# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl #TrackingRef 'shelxl-Pr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H42 Mo N14 O6 Pr' _chemical_formula_weight 883.59 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' Mo Mo -1.6832 0.6857 '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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.280(2) _cell_length_b 16.992(3) _cell_length_c 11.204(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.87(3) _cell_angle_gamma 90.00 _cell_volume 1938.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 890 _exptl_absorpt_coefficient_mu 1.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7593 _exptl_absorpt_correction_T_max 0.8294 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15803 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.0837 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6621 _reflns_number_gt 6058 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.014(18) _refine_ls_number_reflns 6621 _refine_ls_number_parameters 445 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1303 _refine_ls_wR_factor_gt 0.1275 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8478(8) 0.3852(5) 1.4054(8) 0.035(2) Uani 1 1 d . . . C2 C 0.6940(10) 0.2786(6) 1.2829(9) 0.037(2) Uani 1 1 d . . . C3 C 0.9363(14) 0.2886(7) 1.2420(11) 0.040(3) Uani 1 1 d . . . C4 C 0.8619(7) 0.3652(6) 1.0450(6) 0.0306(16) Uani 1 1 d . . . C5 C 0.9640(11) 0.4535(11) 1.2451(9) 0.044(4) Uani 1 1 d . . . C6 C 0.7431(10) 0.4914(6) 1.1221(9) 0.039(2) Uani 1 1 d . . . C7 C 0.6276(11) 0.4342(6) 1.2897(9) 0.042(2) Uani 1 1 d . . . C8 C 0.6247(9) 0.3505(7) 1.0769(8) 0.044(2) Uani 1 1 d . . . C9 C 1.2149(11) 0.2661(8) 0.9448(10) 0.056(3) Uani 1 1 d . . . H9 H 1.2278 0.2147 0.9206 0.067 Uiso 1 1 calc R . . C10 C 1.2466(14) 0.3630(8) 1.0937(11) 0.085(4) Uani 1 1 d D . . H10A H 1.2347 0.3990 1.0271 0.127 Uiso 1 1 calc R . . H10B H 1.3241 0.3771 1.1473 0.127 Uiso 1 1 calc R . . H10C H 1.1717 0.3653 1.1362 0.127 Uiso 1 1 calc R . . C11 C 1.3242(14) 0.2259(10) 1.1321(14) 0.088(5) Uani 1 1 d . . . H11A H 1.3720 0.1899 1.0885 0.131 Uiso 1 1 calc R . . H11B H 1.2589 0.1977 1.1685 0.131 Uiso 1 1 calc R . . H11C H 1.3837 0.2514 1.1937 0.131 Uiso 1 1 calc R . . C12 C 1.2710(13) 0.3636(12) 0.6381(12) 0.082(2) Uani 1 1 d U . . H12 H 1.3138 0.3404 0.7078 0.099 Uiso 1 1 calc R . . C13 C 0.9843(13) 0.2039(6) 0.5556(11) 0.053(3) Uani 1 1 d . . . H13 H 0.9031 0.2191 0.5153 0.063 Uiso 1 1 calc R . . C14 C 1.1628(16) 0.1149(9) 0.5891(16) 0.085(5) Uani 1 1 d . . . H14A H 1.2231 0.1581 0.5895 0.127 Uiso 1 1 calc R . . H14B H 1.1955 0.0707 0.5488 0.127 Uiso 1 1 calc R . . H14C H 1.1540 0.1006 0.6705 0.127 Uiso 1 1 calc R . . C15 C 0.964(2) 0.0896(9) 0.4326(15) 0.099(6) Uani 1 1 d . . . H15A H 0.8924 0.1187 0.3896 0.148 Uiso 1 1 calc R . . H15B H 0.9305 0.0440 0.4688 0.148 Uiso 1 1 calc R . . H15C H 1.0229 0.0735 0.3778 0.148 Uiso 1 1 calc R . . C16 C 0.7001(11) 0.2432(7) 0.7778(11) 0.045(3) Uani 1 1 d . . . H16 H 0.6802 0.2723 0.8432 0.054 Uiso 1 1 calc R . . C17 C 0.5210(14) 0.1567(12) 0.8077(17) 0.101(6) Uani 1 1 d . . . H17A H 0.4962 0.1997 0.8553 0.152 Uiso 1 1 calc R . . H17B H 0.5459 0.1124 0.8590 0.152 Uiso 1 1 calc R . . H17C H 0.4481 0.1424 0.7487 0.152 Uiso 1 1 calc R . . C18 C 0.6654(19) 0.1292(10) 0.6504(18) 0.100(6) Uani 1 1 d . . . H18A H 0.6555 0.1580 0.5760 0.150 Uiso 1 1 calc R . . H18B H 0.6083 0.0843 0.6424 0.150 Uiso 1 1 calc R . . H18C H 0.7548 0.1121 0.6695 0.150 Uiso 1 1 calc R . . C19 C 0.6756(14) 0.4613(8) 0.7808(14) 0.062(4) Uani 1 1 d . . . H19 H 0.6687 0.4364 0.8536 0.074 Uiso 1 1 calc R . . C20 C 0.4746(17) 0.5241(13) 0.8071(16) 0.097(6) Uani 1 1 d . . . H20A H 0.3925 0.5113 0.7595 0.146 Uiso 1 1 calc R . . H20B H 0.4747 0.5785 0.8299 0.146 Uiso 1 1 calc R . . H20C H 0.4862 0.4919 0.8782 0.146 Uiso 1 1 calc R . . C21 C 0.589(2) 0.5576(16) 0.6350(17) 0.157(13) Uani 1 1 d . . . H21A H 0.6781 0.5579 0.6172 0.235 Uiso 1 1 calc R . . H21B H 0.5632 0.6103 0.6513 0.235 Uiso 1 1 calc R . . H21C H 0.5323 0.5370 0.5671 0.235 Uiso 1 1 calc R . . C22 C 1.0119(11) 0.5321(6) 0.9057(10) 0.045(3) Uani 1 1 d . . . H22 H 0.9280 0.5253 0.9261 0.054 Uiso 1 1 calc R . . C23 C 1.0355(17) 0.6398(8) 1.0466(12) 0.079(5) Uani 1 1 d . . . H23A H 1.0591 0.6932 1.0318 0.118 Uiso 1 1 calc R . . H23B H 1.0747 0.6244 1.1259 0.118 Uiso 1 1 calc R . . H23C H 0.9418 0.6356 1.0408 0.118 Uiso 1 1 calc R . . C24 C 1.2092(15) 0.6058(11) 0.9251(18) 0.102(6) Uani 1 1 d . . . H24A H 1.2693 0.5647 0.9541 0.153 Uiso 1 1 calc R . . H24B H 1.2406 0.6551 0.9599 0.153 Uiso 1 1 calc R . . H24C H 1.2026 0.6090 0.8390 0.153 Uiso 1 1 calc R . . C25 C 1.447(2) 0.3198(13) 0.5365(19) 0.120(5) Uani 1 1 d U . . H25A H 1.5099 0.3601 0.5274 0.180 Uiso 1 1 calc R . . H25B H 1.4385 0.2855 0.4678 0.180 Uiso 1 1 calc R . . H25C H 1.4747 0.2900 0.6082 0.180 Uiso 1 1 calc R . . C26 C 1.252(2) 0.3965(14) 0.4379(17) 0.124(5) Uani 1 1 d U . . H26A H 1.2347 0.3587 0.3741 0.186 Uiso 1 1 calc R . . H26B H 1.3100 0.4365 0.4147 0.186 Uiso 1 1 calc R . . H26C H 1.1716 0.4201 0.4533 0.186 Uiso 1 1 calc R . . Mo1 Mo 0.78760(6) 0.38031(4) 1.21491(6) 0.02605(18) Uani 1 1 d . . . N1 N 0.8781(8) 0.3847(5) 1.5103(6) 0.0397(19) Uani 1 1 d . . . N2 N 0.6461(11) 0.2251(7) 1.3223(11) 0.069(3) Uani 1 1 d . . . N3 N 1.0228(13) 0.2454(8) 1.2580(12) 0.071(4) Uani 1 1 d . . . N4 N 0.8990(7) 0.3585(6) 0.9530(6) 0.0396(17) Uani 1 1 d . . . N5 N 1.0531(12) 0.4908(8) 1.2580(10) 0.061(3) Uani 1 1 d . . . N6 N 0.7181(11) 0.5493(6) 1.0697(9) 0.060(3) Uani 1 1 d . . . N7 N 0.5445(11) 0.4647(8) 1.3306(11) 0.077(4) Uani 1 1 d . . . N8 N 0.5451(9) 0.3350(7) 1.0019(8) 0.068(3) Uani 1 1 d . . . N9 N 1.0820(9) 0.5890(5) 0.9588(8) 0.045(2) Uani 1 1 d . . . N10 N 1.2607(8) 0.2848(6) 1.0499(8) 0.051(2) Uani 1 1 d D . . N11 N 1.3144(11) 0.3575(10) 0.5460(10) 0.084(2) Uani 1 1 d U . . N12 N 1.0329(12) 0.1385(5) 0.5249(9) 0.055(3) Uani 1 1 d . . . N13 N 0.6312(10) 0.1802(6) 0.7472(9) 0.057(3) Uani 1 1 d . . . N14 N 0.5812(11) 0.5096(7) 0.7373(11) 0.068(3) Uani 1 1 d . . . O1 O 1.0466(8) 0.4865(4) 0.8311(7) 0.052(2) Uani 1 1 d . . . O2 O 1.1514(8) 0.3124(5) 0.8681(6) 0.060(2) Uani 1 1 d . . . O3 O 1.1576(8) 0.4051(5) 0.6413(7) 0.0634(19) Uani 1 1 d U . . O4 O 1.0375(8) 0.2474(5) 0.6342(8) 0.061(2) Uani 1 1 d . . . O5 O 0.7894(10) 0.2661(6) 0.7247(9) 0.058(3) Uani 1 1 d . . . O6 O 0.7762(10) 0.4466(6) 0.7295(8) 0.056(3) Uani 1 1 d . . . Pr1 Pr 0.97001(4) 0.36411(2) 0.73683(3) 0.02674(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(4) 0.037(5) 0.038(5) -0.002(4) 0.010(4) 0.003(4) C2 0.042(6) 0.036(5) 0.031(5) 0.001(4) 0.003(4) -0.007(4) C3 0.048(7) 0.031(5) 0.040(7) 0.003(4) 0.007(5) 0.000(5) C4 0.035(4) 0.037(4) 0.021(4) 0.007(5) 0.008(3) -0.005(5) C5 0.034(7) 0.085(11) 0.012(5) 0.001(5) 0.004(4) -0.009(6) C6 0.042(5) 0.038(5) 0.038(6) 0.005(4) 0.011(4) 0.003(4) C7 0.047(6) 0.059(6) 0.023(5) 0.010(4) 0.008(4) 0.009(5) C8 0.037(5) 0.067(7) 0.026(4) -0.004(5) -0.002(4) -0.002(5) C9 0.054(7) 0.065(7) 0.050(7) 0.007(6) 0.012(6) 0.001(6) C10 0.089(9) 0.110(11) 0.059(7) -0.013(11) 0.021(6) -0.010(12) C11 0.055(8) 0.104(12) 0.098(12) 0.045(10) -0.009(8) 0.011(8) C12 0.080(3) 0.086(3) 0.084(3) 0.002(3) 0.026(3) 0.003(3) C13 0.067(8) 0.034(6) 0.057(7) -0.013(5) 0.011(6) 0.006(5) C14 0.082(11) 0.064(9) 0.110(14) -0.018(9) 0.017(9) 0.011(8) C15 0.168(19) 0.047(8) 0.076(12) -0.024(8) -0.004(11) -0.010(10) C16 0.040(6) 0.054(6) 0.041(6) -0.003(5) 0.003(5) -0.011(5) C17 0.045(8) 0.130(16) 0.128(15) 0.017(13) 0.009(9) -0.037(10) C18 0.107(13) 0.082(11) 0.114(15) -0.038(10) 0.022(11) -0.037(10) C19 0.071(10) 0.057(7) 0.055(8) 0.012(6) 0.002(7) 0.015(7) C20 0.077(11) 0.142(17) 0.079(12) -0.026(11) 0.032(9) 0.016(11) C21 0.20(2) 0.21(3) 0.080(13) 0.086(15) 0.072(15) 0.14(2) C22 0.054(6) 0.035(5) 0.047(6) -0.011(5) 0.007(5) -0.014(5) C23 0.126(14) 0.051(8) 0.070(10) -0.023(7) 0.055(9) -0.019(8) C24 0.066(10) 0.097(12) 0.150(18) -0.049(12) 0.036(10) -0.024(9) C25 0.116(6) 0.121(6) 0.126(6) 0.006(4) 0.026(4) 0.005(4) C26 0.122(6) 0.125(6) 0.123(6) 0.002(4) 0.010(4) 0.001(4) Mo1 0.0283(3) 0.0334(4) 0.0171(3) 0.0010(3) 0.0056(2) 0.0018(3) N1 0.051(4) 0.052(5) 0.015(3) -0.002(3) 0.000(3) 0.013(4) N2 0.066(7) 0.057(7) 0.082(8) 0.018(6) 0.005(6) -0.014(6) N3 0.056(8) 0.070(8) 0.088(10) 0.015(6) 0.019(7) 0.029(6) N4 0.043(4) 0.046(4) 0.029(4) -0.006(4) 0.003(3) 0.004(5) N5 0.049(7) 0.084(8) 0.047(7) 0.006(5) 0.000(5) -0.026(6) N6 0.073(7) 0.049(5) 0.062(7) 0.020(5) 0.023(5) 0.009(5) N7 0.057(7) 0.108(9) 0.074(8) 0.020(7) 0.039(6) 0.039(7) N8 0.035(5) 0.127(11) 0.045(5) -0.004(6) 0.012(4) -0.019(5) N9 0.055(6) 0.035(4) 0.046(5) -0.005(4) 0.013(4) -0.011(4) N10 0.040(5) 0.077(7) 0.033(5) 0.014(5) -0.003(4) 0.002(4) N11 0.081(3) 0.093(4) 0.082(4) 0.004(3) 0.031(3) 0.008(3) N12 0.087(8) 0.031(5) 0.049(7) -0.004(4) 0.019(6) -0.004(5) N13 0.063(6) 0.051(5) 0.055(6) -0.001(5) 0.008(5) -0.017(5) N14 0.057(7) 0.072(8) 0.077(8) 0.002(6) 0.015(6) 0.029(6) O1 0.081(6) 0.035(4) 0.046(5) -0.012(3) 0.024(4) -0.007(4) O2 0.058(5) 0.082(6) 0.037(4) 0.014(4) -0.005(3) 0.011(4) O3 0.062(3) 0.065(3) 0.068(3) 0.001(3) 0.025(3) 0.002(3) O4 0.068(5) 0.039(4) 0.076(6) -0.032(4) 0.006(4) 0.006(4) O5 0.061(6) 0.058(6) 0.055(6) -0.007(4) 0.005(5) -0.024(4) O6 0.060(6) 0.075(6) 0.035(5) 0.009(4) 0.012(4) 0.043(5) Pr1 0.0357(2) 0.0270(2) 0.0179(2) -0.00147(18) 0.00496(15) 0.0020(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 C1 N1 1.174(11) . ? C1 Mo1 2.141(9) . ? C2 N2 1.150(14) . ? C2 Mo1 2.166(10) . ? C3 N3 1.148(18) . ? C3 Mo1 2.174(13) . ? C4 N4 1.153(9) . ? C4 Mo1 2.162(7) . ? C5 N5 1.107(17) . ? C5 Mo1 2.187(14) . ? C6 N6 1.156(13) . ? C6 Mo1 2.173(10) . ? C7 N7 1.147(14) . ? C7 Mo1 2.150(10) . ? C8 N8 1.121(12) . ? C8 Mo1 2.178(9) . ? C9 N10 1.247(13) . ? C9 O2 1.276(14) . ? C9 H9 0.9300 . ? C10 N10 1.431(9) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N10 1.452(15) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N11 1.183(14) . ? C12 O3 1.367(17) . ? C12 H12 0.9300 . ? C13 O4 1.220(14) . ? C13 N12 1.286(14) . ? C13 H13 0.9300 . ? C14 N12 1.48(2) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N12 1.435(17) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 O5 1.224(15) . ? C16 N13 1.304(15) . ? C16 H16 0.9300 . ? C17 N13 1.453(17) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N13 1.467(18) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O6 1.275(17) . ? C19 N14 1.312(17) . ? C19 H19 0.9300 . ? C20 N14 1.453(19) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N14 1.419(19) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 O1 1.228(12) . ? C22 N9 1.301(13) . ? C22 H22 0.9300 . ? C23 N9 1.438(14) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N9 1.439(17) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N11 1.52(2) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 N11 1.45(2) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? N1 Pr1 2.608(7) 1_556 ? N4 Pr1 2.625(7) . ? O1 Pr1 2.415(7) . ? O2 Pr1 2.379(7) . ? O3 Pr1 2.432(7) . ? O4 Pr1 2.440(7) . ? O5 Pr1 2.484(9) . ? O6 Pr1 2.428(8) . ? Pr1 N1 2.608(7) 1_554 ? 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 N1 C1 Mo1 177.1(8) . . ? N2 C2 Mo1 178.0(10) . . ? N3 C3 Mo1 174.0(14) . . ? N4 C4 Mo1 178.1(9) . . ? N5 C5 Mo1 178.6(10) . . ? N6 C6 Mo1 178.0(10) . . ? N7 C7 Mo1 178.0(12) . . ? N8 C8 Mo1 176.6(8) . . ? N10 C9 O2 124.8(12) . . ? N10 C9 H9 117.6 . . ? O2 C9 H9 117.6 . . ? N10 C10 H10A 109.5 . . ? N10 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N10 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N10 C11 H11A 109.5 . . ? N10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N11 C12 O3 119.5(15) . . ? N11 C12 H12 120.2 . . ? O3 C12 H12 120.2 . . ? O4 C13 N12 124.4(13) . . ? O4 C13 H13 117.8 . . ? N12 C13 H13 117.8 . . ? N12 C14 H14A 109.5 . . ? N12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N12 C15 H15A 109.5 . . ? N12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O5 C16 N13 123.4(12) . . ? O5 C16 H16 118.3 . . ? N13 C16 H16 118.3 . . ? N13 C17 H17A 109.5 . . ? N13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N13 C18 H18A 109.5 . . ? N13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O6 C19 N14 124.0(13) . . ? O6 C19 H19 118.0 . . ? N14 C19 H19 118.0 . . ? N14 C20 H20A 109.5 . . ? N14 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N14 C21 H21A 109.5 . . ? N14 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N14 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O1 C22 N9 125.9(11) . . ? O1 C22 H22 117.0 . . ? N9 C22 H22 117.0 . . ? N9 C23 H23A 109.5 . . ? N9 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N9 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N9 C24 H24A 109.5 . . ? N9 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N9 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N11 C25 H25A 109.5 . . ? N11 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N11 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N11 C26 H26A 109.5 . . ? N11 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N11 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C1 Mo1 C7 74.2(4) . . ? C1 Mo1 C4 142.6(3) . . ? C7 Mo1 C4 140.8(3) . . ? C1 Mo1 C2 76.2(3) . . ? C7 Mo1 C2 78.6(4) . . ? C4 Mo1 C2 116.2(4) . . ? C1 Mo1 C6 117.2(4) . . ? C7 Mo1 C6 72.2(4) . . ? C4 Mo1 C6 76.0(4) . . ? C2 Mo1 C6 141.8(4) . . ? C1 Mo1 C3 77.7(4) . . ? C7 Mo1 C3 144.2(4) . . ? C4 Mo1 C3 73.2(4) . . ? C2 Mo1 C3 73.6(4) . . ? C6 Mo1 C3 141.9(4) . . ? C1 Mo1 C8 143.7(3) . . ? C7 Mo1 C8 79.7(4) . . ? C4 Mo1 C8 71.1(3) . . ? C2 Mo1 C8 74.2(4) . . ? C6 Mo1 C8 76.8(4) . . ? C3 Mo1 C8 112.9(4) . . ? C1 Mo1 C5 72.8(4) . . ? C7 Mo1 C5 111.1(5) . . ? C4 Mo1 C5 79.5(4) . . ? C2 Mo1 C5 143.0(4) . . ? C6 Mo1 C5 72.3(5) . . ? C3 Mo1 C5 80.4(4) . . ? C8 Mo1 C5 141.5(4) . . ? C1 N1 Pr1 170.5(7) . 1_556 ? C4 N4 Pr1 171.7(9) . . ? C22 N9 C23 123.0(11) . . ? C22 N9 C24 119.6(10) . . ? C23 N9 C24 117.4(11) . . ? C9 N10 C10 121.1(10) . . ? C9 N10 C11 120.2(12) . . ? C10 N10 C11 118.6(11) . . ? C12 N11 C26 120.9(16) . . ? C12 N11 C25 123.1(15) . . ? C26 N11 C25 115.4(13) . . ? C13 N12 C15 121.4(12) . . ? C13 N12 C14 117.5(12) . . ? C15 N12 C14 121.1(12) . . ? C16 N13 C17 122.2(12) . . ? C16 N13 C18 120.2(11) . . ? C17 N13 C18 117.6(13) . . ? C19 N14 C21 122.5(13) . . ? C19 N14 C20 118.7(14) . . ? C21 N14 C20 118.1(13) . . ? C22 O1 Pr1 137.2(7) . . ? C9 O2 Pr1 158.2(8) . . ? C12 O3 Pr1 126.5(9) . . ? C13 O4 Pr1 134.7(8) . . ? C16 O5 Pr1 142.3(8) . . ? C19 O6 Pr1 144.2(9) . . ? O2 Pr1 O1 82.3(3) . . ? O2 Pr1 O6 143.5(3) . . ? O1 Pr1 O6 74.6(3) . . ? O2 Pr1 O3 77.1(3) . . ? O1 Pr1 O3 73.5(3) . . ? O6 Pr1 O3 121.1(3) . . ? O2 Pr1 O4 75.0(3) . . ? O1 Pr1 O4 144.0(3) . . ? O6 Pr1 O4 137.6(3) . . ? O3 Pr1 O4 74.4(3) . . ? O2 Pr1 O5 107.6(3) . . ? O1 Pr1 O5 142.9(3) . . ? O6 Pr1 O5 77.4(3) . . ? O3 Pr1 O5 143.1(3) . . ? O4 Pr1 O5 71.8(3) . . ? O2 Pr1 N1 143.2(2) . 1_554 ? O1 Pr1 N1 111.3(3) . 1_554 ? O6 Pr1 N1 72.7(3) . 1_554 ? O3 Pr1 N1 74.7(3) . 1_554 ? O4 Pr1 N1 74.9(3) . 1_554 ? O5 Pr1 N1 82.4(3) . 1_554 ? O2 Pr1 N4 73.1(2) . . ? O1 Pr1 N4 75.1(3) . . ? O6 Pr1 N4 73.8(3) . . ? O3 Pr1 N4 138.9(3) . . ? O4 Pr1 N4 122.6(3) . . ? O5 Pr1 N4 74.1(3) . . ? N1 Pr1 N4 142.5(2) 1_554 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 Mo1 C7 87(14) . . . . ? N1 C1 Mo1 C4 -110(14) . . . . ? N1 C1 Mo1 C2 5(14) . . . . ? N1 C1 Mo1 C6 147(14) . . . . ? N1 C1 Mo1 C3 -71(14) . . . . ? N1 C1 Mo1 C8 41(15) . . . . ? N1 C1 Mo1 C5 -155(14) . . . . ? N7 C7 Mo1 C1 65(29) . . . . ? N7 C7 Mo1 C4 -99(29) . . . . ? N7 C7 Mo1 C2 144(29) . . . . ? N7 C7 Mo1 C6 -61(29) . . . . ? N7 C7 Mo1 C3 104(29) . . . . ? N7 C7 Mo1 C8 -141(29) . . . . ? N7 C7 Mo1 C5 1(29) . . . . ? N4 C4 Mo1 C1 -146(28) . . . . ? N4 C4 Mo1 C7 8(28) . . . . ? N4 C4 Mo1 C2 112(28) . . . . ? N4 C4 Mo1 C6 -29(28) . . . . ? N4 C4 Mo1 C3 174(100) . . . . ? N4 C4 Mo1 C8 52(28) . . . . ? N4 C4 Mo1 C5 -103(28) . . . . ? N2 C2 Mo1 C1 -3(30) . . . . ? N2 C2 Mo1 C7 -79(30) . . . . ? N2 C2 Mo1 C4 139(30) . . . . ? N2 C2 Mo1 C6 -120(30) . . . . ? N2 C2 Mo1 C3 78(30) . . . . ? N2 C2 Mo1 C8 -162(30) . . . . ? N2 C2 Mo1 C5 31(30) . . . . ? N6 C6 Mo1 C1 -173(26) . . . . ? N6 C6 Mo1 C7 -112(26) . . . . ? N6 C6 Mo1 C4 44(26) . . . . ? N6 C6 Mo1 C2 -70(27) . . . . ? N6 C6 Mo1 C3 81(27) . . . . ? N6 C6 Mo1 C8 -29(26) . . . . ? N6 C6 Mo1 C5 128(26) . . . . ? N3 C3 Mo1 C1 -73(11) . . . . ? N3 C3 Mo1 C7 -111(11) . . . . ? N3 C3 Mo1 C4 84(11) . . . . ? N3 C3 Mo1 C2 -152(11) . . . . ? N3 C3 Mo1 C6 46(11) . . . . ? N3 C3 Mo1 C8 144(11) . . . . ? N3 C3 Mo1 C5 2(11) . . . . ? N8 C8 Mo1 C1 -163(19) . . . . ? N8 C8 Mo1 C7 153(19) . . . . ? N8 C8 Mo1 C4 -1(19) . . . . ? N8 C8 Mo1 C2 -126(19) . . . . ? N8 C8 Mo1 C6 79(19) . . . . ? N8 C8 Mo1 C3 -62(19) . . . . ? N8 C8 Mo1 C5 42(19) . . . . ? N5 C5 Mo1 C1 -177(100) . . . . ? N5 C5 Mo1 C7 -112(65) . . . . ? N5 C5 Mo1 C4 28(65) . . . . ? N5 C5 Mo1 C2 149(64) . . . . ? N5 C5 Mo1 C6 -50(65) . . . . ? N5 C5 Mo1 C3 103(65) . . . . ? N5 C5 Mo1 C8 -12(65) . . . . ? Mo1 C1 N1 Pr1 68(16) . . . 1_556 ? Mo1 C4 N4 Pr1 28(32) . . . . ? O1 C22 N9 C23 -179.3(12) . . . . ? O1 C22 N9 C24 4(2) . . . . ? O2 C9 N10 C10 -0.9(18) . . . . ? O2 C9 N10 C11 176.1(12) . . . . ? O3 C12 N11 C26 3(3) . . . . ? O3 C12 N11 C25 173.6(16) . . . . ? O4 C13 N12 C15 179.1(13) . . . . ? O4 C13 N12 C14 0(2) . . . . ? O5 C16 N13 C17 -176.6(14) . . . . ? O5 C16 N13 C18 5(2) . . . . ? O6 C19 N14 C21 -8(3) . . . . ? O6 C19 N14 C20 -177.3(15) . . . . ? N9 C22 O1 Pr1 167.4(8) . . . . ? N10 C9 O2 Pr1 -114(2) . . . . ? N11 C12 O3 Pr1 133.5(15) . . . . ? N12 C13 O4 Pr1 -170.3(8) . . . . ? N13 C16 O5 Pr1 -171.6(10) . . . . ? N14 C19 O6 Pr1 -172.6(11) . . . . ? C9 O2 Pr1 O1 134(2) . . . . ? C9 O2 Pr1 O6 83(2) . . . . ? C9 O2 Pr1 O3 -152(2) . . . . ? C9 O2 Pr1 O4 -74(2) . . . . ? C9 O2 Pr1 O5 -10(2) . . . . ? C9 O2 Pr1 N1 -111(2) . . . 1_554 ? C9 O2 Pr1 N4 57(2) . . . . ? C22 O1 Pr1 O2 -106.0(11) . . . . ? C22 O1 Pr1 O6 45.5(11) . . . . ? C22 O1 Pr1 O3 175.3(12) . . . . ? C22 O1 Pr1 O4 -157.1(10) . . . . ? C22 O1 Pr1 O5 3.2(14) . . . . ? C22 O1 Pr1 N1 109.5(11) . . . 1_554 ? C22 O1 Pr1 N4 -31.5(11) . . . . ? C19 O6 Pr1 O2 -46(2) . . . . ? C19 O6 Pr1 O1 -98.6(17) . . . . ? C19 O6 Pr1 O3 -157.9(16) . . . . ? C19 O6 Pr1 O4 100.9(16) . . . . ? C19 O6 Pr1 O5 56.8(16) . . . . ? C19 O6 Pr1 N1 142.8(18) . . . 1_554 ? C19 O6 Pr1 N4 -20.0(16) . . . . ? C12 O3 Pr1 O2 35.2(11) . . . . ? C12 O3 Pr1 O1 120.9(11) . . . . ? C12 O3 Pr1 O6 -179.2(10) . . . . ? C12 O3 Pr1 O4 -42.6(10) . . . . ? C12 O3 Pr1 O5 -67.0(12) . . . . ? C12 O3 Pr1 N1 -120.8(11) . . . 1_554 ? C12 O3 Pr1 N4 79.4(11) . . . . ? C13 O4 Pr1 O2 158.8(13) . . . . ? C13 O4 Pr1 O1 -148.2(11) . . . . ? C13 O4 Pr1 O6 -1.4(14) . . . . ? C13 O4 Pr1 O3 -120.7(12) . . . . ? C13 O4 Pr1 O5 44.2(12) . . . . ? C13 O4 Pr1 N1 -42.7(12) . . . 1_554 ? C13 O4 Pr1 N4 100.7(12) . . . . ? C16 O5 Pr1 O2 82.1(16) . . . . ? C16 O5 Pr1 O1 -18.8(18) . . . . ? C16 O5 Pr1 O6 -60.4(15) . . . . ? C16 O5 Pr1 O3 173.9(13) . . . . ? C16 O5 Pr1 O4 149.2(16) . . . . ? C16 O5 Pr1 N1 -134.3(16) . . . 1_554 ? C16 O5 Pr1 N4 16.1(15) . . . . ? C4 N4 Pr1 O2 134(5) . . . . ? C4 N4 Pr1 O1 48(5) . . . . ? C4 N4 Pr1 O6 -30(5) . . . . ? C4 N4 Pr1 O3 89(5) . . . . ? C4 N4 Pr1 O4 -166(5) . . . . ? C4 N4 Pr1 O5 -111(5) . . . . ? C4 N4 Pr1 N1 -58(5) . . . 1_554 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.570 _refine_diff_density_min -1.140 _refine_diff_density_rms 0.148 _database_code_depnum_ccdc_archive 'CCDC 889230' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl2 #TrackingRef 'shelxl-Nd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H42 Mo N14 Nd O6' _chemical_formula_weight 886.92 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' Mo Mo -1.6832 0.6857 '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' Nd Nd -0.1943 3.0179 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.257(2) _cell_length_b 16.936(3) _cell_length_c 11.176(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.09(3) _cell_angle_gamma 90.00 _cell_volume 1922.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 1.716 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7475 _exptl_absorpt_correction_T_max 0.8205 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16062 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0939 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6759 _reflns_number_gt 5894 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.124(14) _refine_ls_number_reflns 6759 _refine_ls_number_parameters 445 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1051 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1370(7) 0.0364(6) 0.4562(6) 0.0332(16) Uani 1 1 d . . . C2 C 0.3752(8) 0.0494(8) 0.4228(7) 0.053(3) Uani 1 1 d . . . C3 C 0.3045(9) 0.1245(6) 0.2154(8) 0.041(2) Uani 1 1 d . . . C4 C 0.3730(10) -0.0320(6) 0.2085(8) 0.043(2) Uani 1 1 d . . . C5 C 0.1534(7) 0.0179(5) 0.0902(7) 0.0300(19) Uani 1 1 d . . . C6 C 0.0405(11) -0.0513(10) 0.2543(10) 0.046(4) Uani 1 1 d . . . C7 C 0.0592(13) 0.1122(8) 0.2565(9) 0.041(3) Uani 1 1 d . . . C8 C 0.2597(9) -0.0906(5) 0.3777(9) 0.041(2) Uani 1 1 d . . . C9 C -0.2104(12) -0.2017(8) 0.5739(14) 0.098(5) Uani 1 1 d . . . H9A H -0.2151 -0.1804 0.6527 0.146 Uiso 1 1 calc R . . H9B H -0.2267 -0.2576 0.5745 0.146 Uiso 1 1 calc R . . H9C H -0.2754 -0.1768 0.5159 0.146 Uiso 1 1 calc R . . C10 C -0.0369(15) -0.2394(7) 0.4509(12) 0.089(5) Uani 1 1 d . . . H10A H 0.0479 -0.2225 0.4337 0.134 Uiso 1 1 calc R . . H10B H -0.0991 -0.2374 0.3783 0.134 Uiso 1 1 calc R . . H10C H -0.0308 -0.2926 0.4811 0.134 Uiso 1 1 calc R . . C11 C -0.2125(9) 0.1325(7) 0.5600(10) 0.058(3) Uani 1 1 d . . . H11 H -0.2289 0.1830 0.5867 0.069 Uiso 1 1 calc R . . C12 C -0.3213(13) 0.1741(8) 0.3683(13) 0.097(5) Uani 1 1 d . . . H12A H -0.4121 0.1609 0.3438 0.146 Uiso 1 1 calc R . . H12B H -0.2770 0.1778 0.2984 0.146 Uiso 1 1 calc R . . H12C H -0.3156 0.2239 0.4098 0.146 Uiso 1 1 calc R . . C13 C -0.2472(11) 0.0361(10) 0.4030(9) 0.086(4) Uani 1 1 d . . . H13A H -0.1916 0.0370 0.3407 0.129 Uiso 1 1 calc R . . H13B H -0.3326 0.0163 0.3703 0.129 Uiso 1 1 calc R . . H13C H -0.2089 0.0025 0.4676 0.129 Uiso 1 1 calc R . . C14 C -0.2636(12) 0.0341(10) 0.8594(11) 0.091(2) Uani 1 1 d U . . H14 H -0.3047 0.0541 0.7861 0.109 Uiso 1 1 calc R . . C15 C -0.2690(17) 0.0062(11) 1.0622(16) 0.143(5) Uani 1 1 d U . . H15A H -0.3127 -0.0437 1.0660 0.215 Uiso 1 1 calc R . . H15B H -0.2851 0.0385 1.1292 0.215 Uiso 1 1 calc R . . H15C H -0.1760 -0.0024 1.0658 0.215 Uiso 1 1 calc R . . C16 C -0.4411(17) 0.0825(10) 0.9503(17) 0.141(5) Uani 1 1 d U . . H16A H -0.4595 0.1156 0.8802 0.211 Uiso 1 1 calc R . . H16B H -0.4389 0.1141 1.0219 0.211 Uiso 1 1 calc R . . H16C H -0.5086 0.0431 0.9489 0.211 Uiso 1 1 calc R . . C17 C 0.0165(11) 0.1987(6) 0.9426(9) 0.050(3) Uani 1 1 d . . . H17 H 0.0997 0.1853 0.9816 0.060 Uiso 1 1 calc R . . C18 C 0.0344(18) 0.3139(7) 1.0638(13) 0.101(6) Uani 1 1 d . . . H18A H -0.0255 0.3323 1.1164 0.151 Uiso 1 1 calc R . . H18B H 0.0701 0.3582 1.0258 0.151 Uiso 1 1 calc R . . H18C H 0.1047 0.2850 1.1100 0.151 Uiso 1 1 calc R . . C19 C -0.1632(13) 0.2854(7) 0.9164(14) 0.090(4) Uani 1 1 d . . . H19A H -0.1661 0.2845 0.8301 0.135 Uiso 1 1 calc R . . H19B H -0.1830 0.3376 0.9417 0.135 Uiso 1 1 calc R . . H19C H -0.2269 0.2489 0.9394 0.135 Uiso 1 1 calc R . . C20 C 0.3375(16) 0.2715(8) 0.8515(15) 0.109(6) Uani 1 1 d . . . H20A H 0.2498 0.2920 0.8320 0.164 Uiso 1 1 calc R . . H20B H 0.3990 0.3144 0.8637 0.164 Uiso 1 1 calc R . . H20C H 0.3431 0.2405 0.9240 0.164 Uiso 1 1 calc R . . C21 C 0.4810(11) 0.2438(8) 0.6934(14) 0.092(5) Uani 1 1 d . . . H21A H 0.4994 0.2021 0.6399 0.137 Uiso 1 1 calc R . . H21B H 0.5563 0.2521 0.7534 0.137 Uiso 1 1 calc R . . H21C H 0.4615 0.2915 0.6479 0.137 Uiso 1 1 calc R . . C22 C 0.2995(10) 0.1562(6) 0.7205(11) 0.045(3) Uani 1 1 d . . . H22 H 0.3206 0.1259 0.6566 0.054 Uiso 1 1 calc R . . C23 C 0.3223(13) -0.0600(7) 0.7213(13) 0.069(4) Uani 1 1 d . . . H23 H 0.3296 -0.0344 0.6490 0.082 Uiso 1 1 calc R . . C24 C 0.4085(19) -0.1550(11) 0.8667(14) 0.156(10) Uani 1 1 d . . . H24A H 0.4599 -0.1307 0.9353 0.234 Uiso 1 1 calc R . . H24B H 0.4417 -0.2071 0.8555 0.234 Uiso 1 1 calc R . . H24C H 0.3183 -0.1583 0.8801 0.234 Uiso 1 1 calc R . . C25 C 0.5255(13) -0.1225(10) 0.6932(13) 0.095(5) Uani 1 1 d . . . H25A H 0.5180 -0.0871 0.6254 0.143 Uiso 1 1 calc R . . H25B H 0.5227 -0.1760 0.6648 0.143 Uiso 1 1 calc R . . H25C H 0.6075 -0.1133 0.7442 0.143 Uiso 1 1 calc R . . C26 C -0.0097(11) -0.1296(5) 0.5967(9) 0.050(3) Uani 1 1 d . . . H26 H 0.0751 -0.1228 0.5780 0.060 Uiso 1 1 calc R . . Mo1 Mo 0.21243(6) 0.02147(4) 0.28483(5) 0.02728(18) Uani 1 1 d . . . N1 N 0.1007(6) 0.0445(5) 0.5459(5) 0.0395(16) Uani 1 1 d . . . N2 N -0.0197(10) 0.1574(7) 0.2414(10) 0.063(3) Uani 1 1 d . . . N3 N 0.3520(10) 0.1774(5) 0.1776(9) 0.065(3) Uani 1 1 d . . . N4 N 0.4556(8) 0.0681(6) 0.4981(8) 0.068(3) Uani 1 1 d . . . N5 N -0.0526(10) -0.0901(6) 0.2429(10) 0.062(3) Uani 1 1 d . . . N6 N 0.2819(9) -0.1483(5) 0.4290(9) 0.062(2) Uani 1 1 d . . . N7 N 0.1206(7) 0.0183(4) -0.0120(6) 0.045(2) Uani 1 1 d . . . N8 N 0.4537(9) -0.0628(6) 0.1656(9) 0.072(3) Uani 1 1 d . . . N9 N -0.0804(8) -0.1874(4) 0.5414(7) 0.0427(19) Uani 1 1 d . . . N10 N -0.2600(7) 0.1139(5) 0.4477(7) 0.048(2) Uani 1 1 d . . . N11 N -0.3187(10) 0.0456(8) 0.9502(9) 0.088(2) Uani 1 1 d U . . N12 N -0.0347(10) 0.2632(5) 0.9726(8) 0.055(3) Uani 1 1 d . . . N13 N 0.4169(9) -0.1089(5) 0.7617(9) 0.061(3) Uani 1 1 d . . . N14 N 0.3685(8) 0.2220(5) 0.7522(8) 0.054(2) Uani 1 1 d . . . Nd1 Nd 0.03091(4) 0.03756(2) 0.76256(3) 0.02774(12) Uani 1 1 d . . . O1 O -0.0379(7) 0.1529(4) 0.8646(7) 0.0588(19) Uani 1 1 d . . . O2 O 0.2080(8) 0.1351(5) 0.7748(8) 0.054(2) Uani 1 1 d . . . O3 O 0.2227(8) -0.0441(5) 0.7702(8) 0.050(2) Uani 1 1 d . . . O4 O -0.0461(7) -0.0846(3) 0.6699(6) 0.0531(18) Uani 1 1 d . . . O5 O -0.1490(6) 0.0882(4) 0.6307(6) 0.0580(19) Uani 1 1 d . . . O6 O -0.1548(7) -0.0030(4) 0.8586(7) 0.0655(18) Uani 1 1 d U . . 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 C1 0.045(4) 0.037(4) 0.018(4) 0.004(5) 0.005(3) -0.005(5) C2 0.042(5) 0.096(9) 0.018(4) -0.014(6) -0.005(4) 0.002(6) C3 0.046(6) 0.045(5) 0.029(5) -0.001(4) -0.002(4) 0.006(5) C4 0.050(6) 0.060(6) 0.023(5) 0.004(4) 0.017(5) 0.010(5) C5 0.029(4) 0.037(5) 0.024(4) 0.002(4) 0.005(3) 0.008(3) C6 0.035(7) 0.077(10) 0.025(7) 0.003(5) 0.001(5) -0.002(5) C7 0.060(7) 0.044(6) 0.018(6) 0.013(4) 0.003(5) -0.010(6) C8 0.039(5) 0.044(5) 0.043(6) -0.002(4) 0.017(4) 0.003(4) C9 0.066(9) 0.109(10) 0.122(13) -0.051(10) 0.031(8) -0.038(8) C10 0.136(12) 0.044(7) 0.099(11) -0.037(7) 0.056(10) -0.028(7) C11 0.043(6) 0.078(7) 0.052(7) 0.001(6) 0.007(5) 0.002(5) C12 0.066(8) 0.120(12) 0.102(11) 0.062(9) 0.000(8) 0.019(8) C13 0.089(8) 0.110(10) 0.062(7) -0.020(10) 0.019(6) -0.020(11) C14 0.091(3) 0.095(3) 0.090(3) 0.004(3) 0.025(3) 0.003(3) C15 0.142(6) 0.146(6) 0.139(6) 0.007(4) 0.012(4) 0.009(4) C16 0.137(6) 0.137(6) 0.148(6) 0.004(4) 0.021(4) 0.010(4) C17 0.058(7) 0.047(6) 0.045(6) -0.008(5) 0.011(5) 0.011(5) C18 0.183(17) 0.044(7) 0.069(10) -0.030(7) -0.008(10) -0.003(8) C19 0.101(11) 0.066(8) 0.102(12) -0.018(8) 0.014(9) 0.020(8) C20 0.146(14) 0.078(10) 0.110(13) -0.050(9) 0.042(11) -0.051(10) C21 0.045(7) 0.107(11) 0.120(13) 0.024(9) 0.001(8) -0.040(7) C22 0.043(6) 0.051(6) 0.038(6) -0.005(5) -0.002(5) -0.016(5) C23 0.076(10) 0.075(8) 0.054(8) -0.007(7) 0.002(7) 0.013(7) C24 0.21(2) 0.196(19) 0.065(11) 0.075(12) 0.045(13) 0.135(17) C25 0.072(10) 0.137(14) 0.083(11) -0.026(10) 0.033(8) 0.024(9) C26 0.065(7) 0.035(5) 0.051(6) -0.005(5) 0.014(5) -0.019(5) Mo1 0.0285(3) 0.0376(5) 0.0163(3) 0.0003(3) 0.0053(3) 0.0017(3) N1 0.054(4) 0.040(4) 0.027(3) -0.005(4) 0.016(3) -0.001(4) N2 0.055(7) 0.068(7) 0.071(8) 0.017(5) 0.025(6) 0.031(5) N3 0.072(7) 0.053(6) 0.069(7) 0.016(5) 0.006(5) -0.010(5) N4 0.038(5) 0.120(9) 0.049(6) -0.001(5) 0.014(4) -0.003(5) N5 0.047(6) 0.084(8) 0.052(7) 0.006(5) -0.005(5) -0.012(5) N6 0.064(6) 0.048(5) 0.076(7) 0.022(5) 0.012(5) 0.005(4) N7 0.067(5) 0.049(5) 0.019(3) -0.004(4) 0.009(3) 0.015(4) N8 0.065(7) 0.086(7) 0.071(7) 0.016(6) 0.034(6) 0.030(5) N9 0.055(5) 0.034(4) 0.040(5) -0.008(4) 0.011(4) -0.005(4) N10 0.038(4) 0.071(6) 0.035(5) 0.011(4) 0.001(4) 0.000(4) N11 0.088(3) 0.099(4) 0.085(3) 0.005(3) 0.037(3) 0.013(3) N12 0.085(7) 0.035(5) 0.049(6) 0.001(4) 0.021(5) -0.004(4) N13 0.047(6) 0.069(6) 0.069(7) 0.013(5) 0.012(5) 0.031(5) N14 0.054(6) 0.054(5) 0.053(6) -0.005(4) 0.007(4) -0.017(4) Nd1 0.0361(2) 0.0298(2) 0.01776(19) -0.0012(2) 0.00526(15) 0.0013(2) O1 0.068(5) 0.038(3) 0.072(5) -0.030(4) 0.015(4) 0.007(3) O2 0.065(6) 0.056(5) 0.043(5) -0.007(4) 0.007(4) -0.027(4) O3 0.051(5) 0.064(5) 0.038(5) 0.003(4) 0.015(4) 0.027(4) O4 0.076(5) 0.035(3) 0.053(4) -0.020(3) 0.022(4) -0.016(3) O5 0.052(4) 0.083(5) 0.037(4) 0.007(4) -0.004(3) 0.023(4) O6 0.061(3) 0.069(3) 0.071(3) 0.008(3) 0.024(3) 0.000(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 C1 N1 1.127(8) . ? C1 Mo1 2.178(7) . ? C2 N4 1.138(11) . ? C2 Mo1 2.159(8) . ? C3 N3 1.130(12) . ? C3 Mo1 2.178(10) . ? C4 N8 1.139(11) . ? C4 Mo1 2.158(9) . ? C5 N7 1.144(9) . ? C5 Mo1 2.175(7) . ? C6 N5 1.152(15) . ? C6 Mo1 2.139(13) . ? C7 N2 1.110(16) . ? C7 Mo1 2.189(14) . ? C8 N6 1.139(11) . ? C8 Mo1 2.184(9) . ? C9 N9 1.451(13) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 N9 1.458(12) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O5 1.210(11) . ? C11 N10 1.318(12) . ? C11 H11 0.9300 . ? C12 N10 1.437(13) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N10 1.422(17) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N11 1.244(13) . ? C14 O6 1.282(14) . ? C14 H14 0.9300 . ? C15 N11 1.447(18) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N11 1.402(17) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O1 1.239(11) . ? C17 N12 1.276(12) . ? C17 H17 0.9300 . ? C18 N12 1.441(13) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N12 1.429(16) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N14 1.461(15) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N14 1.454(13) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 O2 1.239(13) . ? C22 N14 1.340(12) . ? C22 H22 0.9300 . ? C23 O3 1.253(15) . ? C23 N13 1.306(14) . ? C23 H23 0.9300 . ? C24 N13 1.423(16) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N13 1.456(15) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O4 1.215(11) . ? C26 N9 1.319(11) . ? C26 H26 0.9300 . ? N1 Nd1 2.622(6) . ? N7 Nd1 2.579(7) 1_554 ? Nd1 O5 2.356(6) . ? Nd1 O3 2.397(7) . ? Nd1 O4 2.398(6) . ? Nd1 O6 2.414(7) . ? Nd1 O1 2.417(6) . ? Nd1 O2 2.444(8) . ? Nd1 N7 2.579(7) 1_556 ? 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 N1 C1 Mo1 178.5(7) . . ? N4 C2 Mo1 175.2(10) . . ? N3 C3 Mo1 178.9(9) . . ? N8 C4 Mo1 176.7(10) . . ? N7 C5 Mo1 177.8(7) . . ? N5 C6 Mo1 177.1(11) . . ? N2 C7 Mo1 179.0(13) . . ? N6 C8 Mo1 177.8(8) . . ? N9 C9 H9A 109.5 . . ? N9 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N9 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N9 C10 H10A 109.5 . . ? N9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 N10 124.5(11) . . ? O5 C11 H11 117.8 . . ? N10 C11 H11 117.8 . . ? N10 C12 H12A 109.5 . . ? N10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N10 C13 H13A 109.5 . . ? N10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N11 C14 O6 125.3(13) . . ? N11 C14 H14 117.4 . . ? O6 C14 H14 117.4 . . ? N11 C15 H15A 109.5 . . ? N11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N11 C16 H16A 109.5 . . ? N11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O1 C17 N12 124.0(10) . . ? O1 C17 H17 118.0 . . ? N12 C17 H17 118.0 . . ? N12 C18 H18A 109.5 . . ? N12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N12 C19 H19A 109.5 . . ? N12 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N12 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N14 C20 H20A 109.5 . . ? N14 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N14 C21 H21A 109.5 . . ? N14 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N14 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O2 C22 N14 121.3(11) . . ? O2 C22 H22 119.4 . . ? N14 C22 H22 119.4 . . ? O3 C23 N13 126.7(14) . . ? O3 C23 H23 116.7 . . ? N13 C23 H23 116.7 . . ? N13 C24 H24A 109.5 . . ? N13 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N13 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N13 C25 H25A 109.5 . . ? N13 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N13 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O4 C26 N9 125.5(10) . . ? O4 C26 H26 117.3 . . ? N9 C26 H26 117.3 . . ? C6 Mo1 C4 110.7(4) . . ? C6 Mo1 C2 141.0(4) . . ? C4 Mo1 C2 79.5(4) . . ? C6 Mo1 C5 73.5(4) . . ? C4 Mo1 C5 73.3(3) . . ? C2 Mo1 C5 143.0(3) . . ? C6 Mo1 C1 79.7(4) . . ? C4 Mo1 C1 141.4(3) . . ? C2 Mo1 C1 71.4(3) . . ? C5 Mo1 C1 143.0(3) . . ? C6 Mo1 C3 142.5(4) . . ? C4 Mo1 C3 78.6(4) . . ? C2 Mo1 C3 75.4(4) . . ? C5 Mo1 C3 74.9(3) . . ? C1 Mo1 C3 116.4(3) . . ? C6 Mo1 C8 72.4(4) . . ? C4 Mo1 C8 72.1(3) . . ? C2 Mo1 C8 75.7(4) . . ? C5 Mo1 C8 117.6(3) . . ? C1 Mo1 C8 76.4(3) . . ? C3 Mo1 C8 141.9(3) . . ? C6 Mo1 C7 79.7(4) . . ? C4 Mo1 C7 144.1(4) . . ? C2 Mo1 C7 114.6(4) . . ? C5 Mo1 C7 77.4(3) . . ? C1 Mo1 C7 73.1(4) . . ? C3 Mo1 C7 74.0(4) . . ? C8 Mo1 C7 141.7(4) . . ? C1 N1 Nd1 169.8(8) . . ? C5 N7 Nd1 172.1(6) . 1_554 ? C26 N9 C9 118.1(9) . . ? C26 N9 C10 124.8(10) . . ? C9 N9 C10 117.1(9) . . ? C11 N10 C13 121.0(9) . . ? C11 N10 C12 119.3(10) . . ? C13 N10 C12 119.6(10) . . ? C14 N11 C16 125.4(14) . . ? C14 N11 C15 119.2(13) . . ? C16 N11 C15 114.3(12) . . ? C17 N12 C19 119.8(10) . . ? C17 N12 C18 121.1(10) . . ? C19 N12 C18 119.1(10) . . ? C23 N13 C24 120.3(12) . . ? C23 N13 C25 120.3(12) . . ? C24 N13 C25 119.1(11) . . ? C22 N14 C21 121.0(10) . . ? C22 N14 C20 120.9(10) . . ? C21 N14 C20 118.0(10) . . ? O5 Nd1 O3 143.1(3) . . ? O5 Nd1 O4 82.1(3) . . ? O3 Nd1 O4 74.7(3) . . ? O5 Nd1 O6 77.5(2) . . ? O3 Nd1 O6 121.0(3) . . ? O4 Nd1 O6 73.4(2) . . ? O5 Nd1 O1 75.3(2) . . ? O3 Nd1 O1 137.9(3) . . ? O4 Nd1 O1 143.3(2) . . ? O6 Nd1 O1 73.7(2) . . ? O5 Nd1 O2 107.4(3) . . ? O3 Nd1 O2 77.8(3) . . ? O4 Nd1 O2 143.5(3) . . ? O6 Nd1 O2 142.5(3) . . ? O1 Nd1 O2 72.0(3) . . ? O5 Nd1 N7 142.9(2) . 1_556 ? O3 Nd1 N7 73.4(2) . 1_556 ? O4 Nd1 N7 111.3(2) . 1_556 ? O6 Nd1 N7 74.0(2) . 1_556 ? O1 Nd1 N7 74.3(2) . 1_556 ? O2 Nd1 N7 82.6(3) . 1_556 ? O5 Nd1 N1 72.4(2) . . ? O3 Nd1 N1 74.3(3) . . ? O4 Nd1 N1 75.9(2) . . ? O6 Nd1 N1 139.3(2) . . ? O1 Nd1 N1 122.4(3) . . ? O2 Nd1 N1 74.0(3) . . ? N7 Nd1 N1 143.3(2) 1_556 . ? C17 O1 Nd1 134.9(7) . . ? C22 O2 Nd1 140.9(7) . . ? C23 O3 Nd1 145.5(9) . . ? C26 O4 Nd1 136.0(6) . . ? C11 O5 Nd1 159.4(7) . . ? C14 O6 Nd1 127.3(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 C6 Mo1 C4 132(26) . . . . ? N5 C6 Mo1 C2 33(27) . . . . ? N5 C6 Mo1 C5 -164(26) . . . . ? N5 C6 Mo1 C1 -9(26) . . . . ? N5 C6 Mo1 C3 -130(26) . . . . ? N5 C6 Mo1 C8 70(26) . . . . ? N5 C6 Mo1 C7 -84(26) . . . . ? N8 C4 Mo1 C6 9(16) . . . . ? N8 C4 Mo1 C2 150(16) . . . . ? N8 C4 Mo1 C5 -56(16) . . . . ? N8 C4 Mo1 C1 108(15) . . . . ? N8 C4 Mo1 C3 -133(16) . . . . ? N8 C4 Mo1 C8 71(16) . . . . ? N8 C4 Mo1 C7 -93(16) . . . . ? N4 C2 Mo1 C6 -90(12) . . . . ? N4 C2 Mo1 C4 160(12) . . . . ? N4 C2 Mo1 C5 117(11) . . . . ? N4 C2 Mo1 C1 -46(12) . . . . ? N4 C2 Mo1 C3 79(12) . . . . ? N4 C2 Mo1 C8 -126(12) . . . . ? N4 C2 Mo1 C7 15(12) . . . . ? N7 C5 Mo1 C6 101(19) . . . . ? N7 C5 Mo1 C4 -141(19) . . . . ? N7 C5 Mo1 C2 -96(19) . . . . ? N7 C5 Mo1 C1 56(19) . . . . ? N7 C5 Mo1 C3 -58(19) . . . . ? N7 C5 Mo1 C8 161(19) . . . . ? N7 C5 Mo1 C7 18(19) . . . . ? N1 C1 Mo1 C6 155(36) . . . . ? N1 C1 Mo1 C4 45(36) . . . . ? N1 C1 Mo1 C2 2(36) . . . . ? N1 C1 Mo1 C5 -161(36) . . . . ? N1 C1 Mo1 C3 -61(36) . . . . ? N1 C1 Mo1 C8 81(36) . . . . ? N1 C1 Mo1 C7 -122(36) . . . . ? N3 C3 Mo1 C6 -54(46) . . . . ? N3 C3 Mo1 C4 55(46) . . . . ? N3 C3 Mo1 C2 137(46) . . . . ? N3 C3 Mo1 C5 -20(46) . . . . ? N3 C3 Mo1 C1 -163(46) . . . . ? N3 C3 Mo1 C8 95(46) . . . . ? N3 C3 Mo1 C7 -101(46) . . . . ? N6 C8 Mo1 C6 -75(24) . . . . ? N6 C8 Mo1 C4 166(24) . . . . ? N6 C8 Mo1 C2 82(24) . . . . ? N6 C8 Mo1 C5 -135(23) . . . . ? N6 C8 Mo1 C1 8(23) . . . . ? N6 C8 Mo1 C3 124(23) . . . . ? N6 C8 Mo1 C7 -30(24) . . . . ? N2 C7 Mo1 C6 -19(64) . . . . ? N2 C7 Mo1 C4 93(65) . . . . ? N2 C7 Mo1 C2 -161(65) . . . . ? N2 C7 Mo1 C5 57(65) . . . . ? N2 C7 Mo1 C1 -101(65) . . . . ? N2 C7 Mo1 C3 134(65) . . . . ? N2 C7 Mo1 C8 -62(65) . . . . ? Mo1 C1 N1 Nd1 -82(37) . . . . ? Mo1 C5 N7 Nd1 -4(23) . . . 1_554 ? O4 C26 N9 C9 -3.1(17) . . . . ? O4 C26 N9 C10 177.9(11) . . . . ? O5 C11 N10 C13 4.5(15) . . . . ? O5 C11 N10 C12 -173.1(11) . . . . ? O6 C14 N11 C16 -176.5(14) . . . . ? O6 C14 N11 C15 -9(2) . . . . ? O1 C17 N12 C19 1.0(18) . . . . ? O1 C17 N12 C18 -179.7(11) . . . . ? O3 C23 N13 C24 5(2) . . . . ? O3 C23 N13 C25 178.8(12) . . . . ? O2 C22 N14 C21 176.0(11) . . . . ? O2 C22 N14 C20 -0.5(18) . . . . ? C1 N1 Nd1 O5 -132(4) . . . . ? C1 N1 Nd1 O3 32(4) . . . . ? C1 N1 Nd1 O4 -46(4) . . . . ? C1 N1 Nd1 O6 -88(4) . . . . ? C1 N1 Nd1 O1 169(3) . . . . ? C1 N1 Nd1 O2 113(4) . . . . ? C1 N1 Nd1 N7 61(4) . . . 1_556 ? N12 C17 O1 Nd1 170.2(8) . . . . ? O5 Nd1 O1 C17 -156.1(10) . . . . ? O3 Nd1 O1 C17 4.3(12) . . . . ? O4 Nd1 O1 C17 150.0(9) . . . . ? O6 Nd1 O1 C17 122.8(10) . . . . ? O2 Nd1 O1 C17 -41.9(10) . . . . ? N7 Nd1 O1 C17 45.3(10) 1_556 . . . ? N1 Nd1 O1 C17 -98.6(10) . . . . ? N14 C22 O2 Nd1 172.0(8) . . . . ? O5 Nd1 O2 C22 -84.0(13) . . . . ? O3 Nd1 O2 C22 58.2(12) . . . . ? O4 Nd1 O2 C22 16.6(15) . . . . ? O6 Nd1 O2 C22 -176.1(11) . . . . ? O1 Nd1 O2 C22 -151.5(13) . . . . ? N7 Nd1 O2 C22 132.7(13) 1_556 . . . ? N1 Nd1 O2 C22 -18.8(12) . . . . ? N13 C23 O3 Nd1 173.9(9) . . . . ? O5 Nd1 O3 C23 45.6(16) . . . . ? O4 Nd1 O3 C23 98.7(15) . . . . ? O6 Nd1 O3 C23 158.0(14) . . . . ? O1 Nd1 O3 C23 -101.8(14) . . . . ? O2 Nd1 O3 C23 -57.1(14) . . . . ? N7 Nd1 O3 C23 -143.0(15) 1_556 . . . ? N1 Nd1 O3 C23 19.4(14) . . . . ? N9 C26 O4 Nd1 -167.0(7) . . . . ? O5 Nd1 O4 C26 106.3(10) . . . . ? O3 Nd1 O4 C26 -44.7(10) . . . . ? O6 Nd1 O4 C26 -174.4(11) . . . . ? O1 Nd1 O4 C26 158.4(9) . . . . ? O2 Nd1 O4 C26 -2.4(12) . . . . ? N7 Nd1 O4 C26 -109.5(10) 1_556 . . . ? N1 Nd1 O4 C26 32.6(10) . . . . ? N10 C11 O5 Nd1 116.8(19) . . . . ? O3 Nd1 O5 C11 -89(2) . . . . ? O4 Nd1 O5 C11 -140(2) . . . . ? O6 Nd1 O5 C11 145(2) . . . . ? O1 Nd1 O5 C11 69(2) . . . . ? O2 Nd1 O5 C11 4(2) . . . . ? N7 Nd1 O5 C11 105(2) 1_556 . . . ? N1 Nd1 O5 C11 -62(2) . . . . ? N11 C14 O6 Nd1 -133.4(14) . . . . ? O5 Nd1 O6 C14 -33.2(10) . . . . ? O3 Nd1 O6 C14 -178.5(9) . . . . ? O4 Nd1 O6 C14 -118.6(10) . . . . ? O1 Nd1 O6 C14 44.9(10) . . . . ? O2 Nd1 O6 C14 69.2(11) . . . . ? N7 Nd1 O6 C14 122.8(10) 1_556 . . . ? N1 Nd1 O6 C14 -76.1(10) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.382 _refine_diff_density_min -0.987 _refine_diff_density_rms 0.116 _database_code_depnum_ccdc_archive 'CCDC 875833' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelx-Sm #TrackingRef 'shelx-Sm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H42 Mo N14 O6 Sm' _chemical_formula_weight 893.04 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' Mo Mo -1.6832 0.6857 '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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.680(3) _cell_length_b 11.190(2) _cell_length_c 21.330(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.58(3) _cell_angle_gamma 90.00 _cell_volume 3979.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1791 _exptl_absorpt_coefficient_mu 1.829 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6891 _exptl_absorpt_correction_T_max 0.8104 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24435 _diffrn_reflns_av_R_equivalents 0.1523 _diffrn_reflns_av_sigmaI/netI 0.1204 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6761 _reflns_number_gt 5092 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1299P)^2^+25.8794P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6761 _refine_ls_number_parameters 445 _refine_ls_number_restraints 140 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.2410 _refine_ls_wR_factor_gt 0.2163 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.062 _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 C1 C 0.2418(7) -0.0865(9) 0.3322(5) 0.055(3) Uani 1 1 d . . . C2 C 0.3598(9) -0.1910(13) 0.3976(7) 0.078(4) Uani 1 1 d . . . C3 C 0.2043(11) -0.1720(12) 0.4386(7) 0.082(4) Uani 1 1 d . . . C4 C 0.2955(9) -0.3841(12) 0.4385(6) 0.073(4) Uani 1 1 d . . . C5 C 0.1403(9) -0.3581(13) 0.3923(6) 0.074(4) Uani 1 1 d . . . C6 C 0.2578(6) -0.4586(9) 0.3270(5) 0.045(2) Uani 1 1 d . . . C7 C 0.1685(9) -0.2700(11) 0.2808(7) 0.063(3) Uani 1 1 d . . . C8 C 0.3326(8) -0.2688(11) 0.2826(6) 0.060(3) Uani 1 1 d . . . C9 C 0.2140(10) 0.0082(14) 0.1717(7) 0.085(3) Uani 1 1 d U . . H9 H 0.2473 -0.0383 0.1975 0.101 Uiso 1 1 calc R . . C10 C 0.4140(7) 0.0575(11) 0.2558(6) 0.061(3) Uani 1 1 d . . . H10 H 0.4086 0.0346 0.2973 0.073 Uiso 1 1 calc R . . C11 C 0.3746(8) 0.2867(11) 0.4002(6) 0.065(3) Uani 1 1 d . . . H11 H 0.3410 0.3475 0.4135 0.078 Uiso 1 1 calc R . . C12 C 0.5014(11) 0.171(2) 0.4088(11) 0.140(9) Uani 1 1 d . . . H12A H 0.4708 0.1049 0.3924 0.210 Uiso 1 1 calc R . . H12C H 0.5352 0.1444 0.4431 0.210 Uiso 1 1 calc R . . H12B H 0.5339 0.2035 0.3765 0.210 Uiso 1 1 calc R . . C13 C 0.4685(14) 0.3427(19) 0.4851(10) 0.131(8) Uani 1 1 d . . . H13A H 0.4217 0.3788 0.5022 0.197 Uiso 1 1 calc R . . H13B H 0.5042 0.4041 0.4714 0.197 Uiso 1 1 calc R . . H13C H 0.4952 0.2949 0.5167 0.197 Uiso 1 1 calc R . . C14 C 0.3380(16) 0.410(2) 0.0340(10) 0.141(7) Uani 1 1 d U . . H14C H 0.3798 0.4674 0.0269 0.212 Uiso 1 1 calc R . . H14A H 0.2954 0.4216 0.0035 0.212 Uiso 1 1 calc R . . H14B H 0.3592 0.3310 0.0304 0.212 Uiso 1 1 calc R . . C15 C 0.2831(15) 0.5405(19) 0.1140(9) 0.120(6) Uani 1 1 d U . . H15B H 0.2936 0.5520 0.1581 0.180 Uiso 1 1 calc R . . H15A H 0.2267 0.5496 0.1050 0.180 Uiso 1 1 calc R . . H15C H 0.3124 0.5988 0.0908 0.180 Uiso 1 1 calc R . . C16 C 0.3041(11) 0.3300(14) 0.1377(8) 0.092(5) Uani 1 1 d . . . H16 H 0.3166 0.2541 0.1233 0.111 Uiso 1 1 calc R . . C17 C 0.1491(15) 0.034(2) 0.0721(10) 0.139(7) Uani 1 1 d U . . H17A H 0.1037 -0.0083 0.0549 0.208 Uiso 1 1 calc R . . H17C H 0.1857 0.0520 0.0393 0.208 Uiso 1 1 calc R . . H17B H 0.1314 0.1077 0.0906 0.208 Uiso 1 1 calc R . . C18 C 0.2192(14) -0.1682(18) 0.1052(9) 0.115(5) Uani 1 1 d U . . H18C H 0.2664 -0.1871 0.1300 0.173 Uiso 1 1 calc R . . H18A H 0.2313 -0.1722 0.0615 0.173 Uiso 1 1 calc R . . H18B H 0.1776 -0.2245 0.1140 0.173 Uiso 1 1 calc R . . C19 C 0.4920(12) 0.056(2) 0.1611(8) 0.111(6) Uani 1 1 d . . . H19B H 0.5152 -0.0080 0.1375 0.166 Uiso 1 1 calc R . . H19C H 0.5289 0.1215 0.1637 0.166 Uiso 1 1 calc R . . H19A H 0.4430 0.0814 0.1406 0.166 Uiso 1 1 calc R . . C20 C 0.5315(8) -0.0667(15) 0.2587(8) 0.089(5) Uani 1 1 d . . . H20B H 0.5127 -0.0823 0.3000 0.134 Uiso 1 1 calc R . . H20C H 0.5833 -0.0293 0.2617 0.134 Uiso 1 1 calc R . . H20A H 0.5357 -0.1407 0.2362 0.134 Uiso 1 1 calc R . . C21 C 0.0874(11) 0.3943(18) 0.2496(12) 0.128(8) Uani 1 1 d . . . H21 H 0.1003 0.4382 0.2855 0.153 Uiso 1 1 calc R . . C22 C 0.013(2) 0.406(5) 0.1535(9) 0.30(3) Uani 1 1 d D . . H22A H 0.0502 0.3460 0.1407 0.454 Uiso 1 1 calc R . . H22C H 0.0169 0.4747 0.1270 0.454 Uiso 1 1 calc R . . H22B H -0.0407 0.3742 0.1501 0.454 Uiso 1 1 calc R . . C23 C 0.1410(14) 0.186(2) 0.4075(11) 0.124(4) Uani 1 1 d U . . H23 H 0.1599 0.1097 0.4161 0.148 Uiso 1 1 calc R . . C24 C -0.0164(17) 0.536(3) 0.2420(15) 0.182(14) Uani 1 1 d . . . H24B H -0.0299 0.5189 0.2845 0.273 Uiso 1 1 calc R . . H24A H -0.0647 0.5448 0.2168 0.273 Uiso 1 1 calc R . . H24C H 0.0140 0.6087 0.2407 0.273 Uiso 1 1 calc R . . C25 C 0.066(2) 0.137(3) 0.4919(13) 0.183(9) Uani 1 1 d DU . . H25C H 0.0938 0.1544 0.5309 0.275 Uiso 1 1 calc R . . H25A H 0.0818 0.0597 0.4773 0.275 Uiso 1 1 calc R . . H25B H 0.0093 0.1382 0.4981 0.275 Uiso 1 1 calc R . . C26 C 0.017(2) 0.319(3) 0.4374(17) 0.202(9) Uani 1 1 d U . . H26A H -0.0292 0.2810 0.4188 0.303 Uiso 1 1 calc R . . H26B H 0.0342 0.3827 0.4105 0.303 Uiso 1 1 calc R . . H26C H 0.0038 0.3518 0.4775 0.303 Uiso 1 1 calc R . . Mo1 Mo 0.24960(6) -0.27335(7) 0.36135(4) 0.0451(3) Uani 1 1 d . . . N1 N 0.2383(6) 0.0139(8) 0.3159(4) 0.052(2) Uani 1 1 d . . . N2 N 0.1733(11) -0.1164(14) 0.4796(6) 0.108(5) Uani 1 1 d . . . N3 N 0.4173(10) -0.1433(16) 0.4135(8) 0.117(5) Uani 1 1 d . . . N4 N 0.3179(10) -0.4433(12) 0.4778(6) 0.100(5) Uani 1 1 d . . . N5 N 0.0792(9) -0.4016(16) 0.4077(7) 0.113(5) Uani 1 1 d . . . N6 N 0.2602(6) -0.5562(8) 0.3119(5) 0.058(2) Uani 1 1 d . . . N7 N 0.3731(10) -0.2673(12) 0.2387(7) 0.092(4) Uani 1 1 d . . . N8 N 0.1255(9) -0.2664(13) 0.2378(7) 0.096(4) Uani 1 1 d . . . N9 N 0.4447(7) 0.2669(11) 0.4316(6) 0.077(3) Uani 1 1 d . . . N10 N 0.1907(9) -0.0408(13) 0.1213(6) 0.097(3) Uani 1 1 d U . . N11 N 0.0862(14) 0.2262(19) 0.4461(10) 0.138(5) Uani 1 1 d DU . . N12 N 0.0305(7) 0.4395(13) 0.2178(7) 0.095(4) Uani 1 1 d D . . N13 N 0.3071(9) 0.4274(13) 0.0971(6) 0.091(3) Uani 1 1 d U . . N14 N 0.4748(8) 0.0129(11) 0.2252(6) 0.080(3) Uani 1 1 d . . . O1 O 0.3635(5) 0.1278(9) 0.2331(4) 0.072(2) Uani 1 1 d . . . O2 O 0.1994(6) 0.1079(8) 0.1918(4) 0.078(2) Uani 1 1 d U . . O3 O 0.2850(7) 0.3436(8) 0.1926(4) 0.078(3) Uani 1 1 d . . . O4 O 0.1274(7) 0.3100(11) 0.2443(7) 0.116(5) Uani 1 1 d . . . O5 O 0.1686(7) 0.2324(10) 0.3650(6) 0.090(3) Uani 1 1 d U . . O6 O 0.3539(5) 0.2256(7) 0.3540(5) 0.067(2) Uani 1 1 d . . . Sm1 Sm 0.24910(3) 0.22528(4) 0.27689(2) 0.0366(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.066(7) 0.025(5) 0.074(7) -0.006(5) -0.002(5) -0.003(5) C2 0.080(9) 0.065(8) 0.087(9) -0.004(7) -0.035(8) -0.008(7) C3 0.122(13) 0.044(7) 0.080(9) 0.009(7) 0.016(8) 0.001(8) C4 0.098(11) 0.055(8) 0.065(7) 0.004(6) -0.008(7) 0.014(7) C5 0.082(10) 0.064(8) 0.077(8) -0.004(6) 0.025(7) 0.004(7) C6 0.054(6) 0.024(5) 0.058(6) 0.001(4) -0.006(5) 0.001(4) C7 0.065(8) 0.047(7) 0.077(8) -0.002(6) -0.014(6) 0.002(6) C8 0.060(7) 0.054(7) 0.065(7) -0.006(5) 0.009(6) -0.005(6) C9 0.099(6) 0.069(5) 0.085(5) -0.014(5) -0.009(5) 0.004(5) C10 0.046(6) 0.048(7) 0.091(8) -0.008(6) 0.018(6) 0.010(5) C11 0.072(8) 0.048(7) 0.075(8) 0.002(6) -0.015(6) -0.004(6) C12 0.070(11) 0.18(2) 0.163(19) -0.022(18) -0.060(12) 0.032(13) C13 0.159(19) 0.104(14) 0.125(14) -0.023(12) -0.089(14) -0.003(13) C14 0.161(13) 0.136(12) 0.128(11) 0.007(11) 0.025(11) 0.007(11) C15 0.147(12) 0.101(11) 0.112(10) 0.008(9) 0.012(10) -0.003(10) C16 0.128(14) 0.055(9) 0.094(11) -0.007(8) 0.010(9) 0.028(9) C17 0.144(12) 0.143(12) 0.128(11) -0.018(11) -0.019(10) 0.002(11) C18 0.151(12) 0.091(10) 0.104(10) 0.001(9) 0.007(9) 0.002(10) C19 0.103(14) 0.140(17) 0.092(11) -0.006(11) 0.039(10) 0.010(12) C20 0.047(7) 0.077(10) 0.144(14) 0.010(9) 0.006(8) 0.008(7) C21 0.077(12) 0.093(14) 0.21(2) 0.027(14) -0.033(13) 0.018(11) C22 0.20(4) 0.60(10) 0.104(19) 0.05(4) -0.03(2) 0.00(5) C23 0.127(7) 0.118(7) 0.128(7) -0.002(6) 0.032(6) 0.005(6) C24 0.14(2) 0.14(2) 0.27(4) -0.10(3) 0.02(2) 0.014(18) C25 0.189(14) 0.171(14) 0.190(14) 0.018(13) 0.005(13) -0.015(13) C26 0.189(15) 0.197(15) 0.220(15) 0.007(13) 0.005(13) 0.001(13) Mo1 0.0648(6) 0.0265(5) 0.0437(5) 0.0003(3) -0.0034(4) 0.0005(4) N1 0.060(6) 0.036(5) 0.060(5) -0.005(4) -0.007(4) 0.005(4) N2 0.146(14) 0.101(11) 0.080(8) -0.026(8) 0.023(8) 0.020(10) N3 0.104(11) 0.116(12) 0.128(12) 0.023(10) -0.055(9) -0.015(10) N4 0.144(14) 0.076(9) 0.080(8) 0.021(7) -0.016(8) 0.033(9) N5 0.088(10) 0.127(14) 0.125(11) 0.002(10) 0.041(9) -0.020(9) N6 0.060(6) 0.033(5) 0.080(6) 0.003(4) -0.007(5) 0.000(4) N7 0.107(11) 0.068(8) 0.101(10) -0.001(7) 0.005(9) -0.016(7) N8 0.104(10) 0.101(10) 0.080(8) 0.018(7) -0.033(8) -0.035(8) N9 0.068(7) 0.072(7) 0.090(8) -0.002(6) -0.037(6) -0.001(6) N10 0.111(6) 0.089(6) 0.090(6) -0.019(5) -0.012(5) 0.004(5) N11 0.138(7) 0.138(7) 0.140(7) 0.003(6) 0.035(6) 0.010(6) N12 0.037(6) 0.101(10) 0.147(12) 0.020(9) -0.030(7) 0.009(6) N13 0.105(7) 0.084(7) 0.085(6) 0.007(5) 0.009(5) 0.006(6) N14 0.076(8) 0.062(7) 0.102(8) -0.009(6) 0.008(6) 0.007(6) O1 0.051(5) 0.085(6) 0.081(5) 0.010(5) 0.012(4) 0.015(5) O2 0.090(5) 0.061(5) 0.082(5) -0.021(4) -0.022(4) 0.009(4) O3 0.115(8) 0.057(6) 0.062(5) 0.004(4) 0.013(5) -0.004(5) O4 0.078(7) 0.084(8) 0.183(13) -0.042(8) -0.050(8) 0.037(7) O5 0.099(6) 0.075(5) 0.100(6) -0.002(4) 0.051(5) -0.002(5) O6 0.062(5) 0.053(5) 0.086(6) -0.011(4) -0.028(4) 0.002(4) Sm1 0.0390(3) 0.0222(3) 0.0484(3) -0.00045(17) -0.0027(2) 0.00245(17) _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 C1 N1 1.177(14) . ? C1 Mo1 2.184(11) . ? C2 N3 1.142(19) . ? C2 Mo1 2.178(14) . ? C3 N2 1.202(18) . ? C3 Mo1 2.154(15) . ? C4 N4 1.125(16) . ? C4 Mo1 2.181(13) . ? C5 N5 1.184(18) . ? C5 Mo1 2.173(15) . ? C6 N6 1.140(13) . ? C6 Mo1 2.204(10) . ? C7 N8 1.149(18) . ? C7 Mo1 2.158(13) . ? C8 N7 1.169(19) . ? C8 Mo1 2.207(13) . ? C9 O2 1.221(17) . ? C9 N10 1.260(18) . ? C9 H9 0.9300 . ? C10 O1 1.242(15) . ? C10 N14 1.319(16) . ? C10 H10 0.9300 . ? C11 O6 1.240(15) . ? C11 N9 1.351(17) . ? C11 H11 0.9300 . ? C12 N9 1.52(2) . ? C12 H12A 0.9600 . ? C12 H12C 0.9600 . ? C12 H12B 0.9600 . ? C13 N9 1.468(19) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N13 1.47(2) . ? C14 H14C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C15 N13 1.38(2) . ? C15 H15B 0.9600 . ? C15 H15A 0.9600 . ? C15 H15C 0.9600 . ? C16 O3 1.230(17) . ? C16 N13 1.39(2) . ? C16 H16 0.9300 . ? C17 N10 1.50(3) . ? C17 H17A 0.9600 . ? C17 H17C 0.9600 . ? C17 H17B 0.9600 . ? C18 N10 1.54(2) . ? C18 H18C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C19 N14 1.48(2) . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C19 H19A 0.9600 . ? C20 N14 1.47(2) . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C20 H20A 0.9600 . ? C21 O4 1.16(2) . ? C21 N12 1.26(2) . ? C21 H21 0.9300 . ? C22 N12 1.444(10) . ? C22 H22A 0.9601 . ? C22 H22C 0.9601 . ? C22 H22B 0.9601 . ? C23 O5 1.15(2) . ? C23 N11 1.32(3) . ? C23 H23 0.9300 . ? C24 N12 1.44(3) . ? C24 H24B 0.9600 . ? C24 H24A 0.9600 . ? C24 H24C 0.9600 . ? C25 N11 1.441(10) . ? C25 H25C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C26 N11 1.56(4) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? N1 Sm1 2.515(9) . ? N6 Sm1 2.562(9) 1_545 ? O1 Sm1 2.408(8) . ? O2 Sm1 2.372(8) . ? O3 Sm1 2.325(9) . ? O4 Sm1 2.328(10) . ? O5 Sm1 2.340(10) . ? O6 Sm1 2.367(8) . ? Sm1 N6 2.562(9) 1_565 ? 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 N1 C1 Mo1 179.2(11) . . ? N3 C2 Mo1 175.9(15) . . ? N2 C3 Mo1 175.0(16) . . ? N4 C4 Mo1 178.3(15) . . ? N5 C5 Mo1 177.6(15) . . ? N6 C6 Mo1 176.6(10) . . ? N8 C7 Mo1 178.9(12) . . ? N7 C8 Mo1 176.3(13) . . ? O2 C9 N10 129.5(16) . . ? O2 C9 H9 115.2 . . ? N10 C9 H9 115.2 . . ? O1 C10 N14 124.8(13) . . ? O1 C10 H10 117.6 . . ? N14 C10 H10 117.6 . . ? O6 C11 N9 121.5(13) . . ? O6 C11 H11 119.2 . . ? N9 C11 H11 119.2 . . ? N9 C12 H12A 109.5 . . ? N9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? N9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? H12C C12 H12B 109.5 . . ? N9 C13 H13A 109.5 . . ? N9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N13 C14 H14C 109.5 . . ? N13 C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? N13 C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N13 C15 H15B 109.5 . . ? N13 C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? N13 C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? O3 C16 N13 120.6(13) . . ? O3 C16 H16 119.7 . . ? N13 C16 H16 119.7 . . ? N10 C17 H17A 109.5 . . ? N10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? N10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? H17C C17 H17B 109.5 . . ? N10 C18 H18C 109.5 . . ? N10 C18 H18A 109.5 . . ? H18C C18 H18A 109.5 . . ? N10 C18 H18B 109.5 . . ? H18C C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N14 C19 H19B 109.5 . . ? N14 C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N14 C19 H19A 109.5 . . ? H19B C19 H19A 109.5 . . ? H19C C19 H19A 109.5 . . ? N14 C20 H20B 109.5 . . ? N14 C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N14 C20 H20A 109.5 . . ? H20B C20 H20A 109.5 . . ? H20C C20 H20A 109.5 . . ? O4 C21 N12 134(3) . . ? O4 C21 H21 112.8 . . ? N12 C21 H21 112.8 . . ? N12 C22 H22A 109.5 . . ? N12 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? N12 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? H22C C22 H22B 109.5 . . ? O5 C23 N11 130(2) . . ? O5 C23 H23 115.2 . . ? N11 C23 H23 115.2 . . ? N12 C24 H24B 109.5 . . ? N12 C24 H24A 109.5 . . ? H24B C24 H24A 109.5 . . ? N12 C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? N11 C25 H25C 109.5 . . ? N11 C25 H25A 109.5 . . ? H25C C25 H25A 109.5 . . ? N11 C25 H25B 109.5 . . ? H25C C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N11 C26 H26A 109.5 . . ? N11 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N11 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C3 Mo1 C7 112.0(6) . . ? C3 Mo1 C5 71.5(6) . . ? C7 Mo1 C5 74.7(6) . . ? C3 Mo1 C2 79.4(7) . . ? C7 Mo1 C2 141.2(6) . . ? C5 Mo1 C2 141.6(6) . . ? C3 Mo1 C4 81.1(5) . . ? C7 Mo1 C4 144.1(5) . . ? C5 Mo1 C4 78.7(6) . . ? C2 Mo1 C4 72.4(6) . . ? C3 Mo1 C1 72.3(5) . . ? C7 Mo1 C1 74.1(4) . . ? C5 Mo1 C1 117.4(5) . . ? C2 Mo1 C1 74.9(5) . . ? C4 Mo1 C1 140.9(5) . . ? C3 Mo1 C6 140.9(5) . . ? C7 Mo1 C6 78.1(4) . . ? C5 Mo1 C6 75.6(5) . . ? C2 Mo1 C6 117.2(5) . . ? C4 Mo1 C6 72.1(4) . . ? C1 Mo1 C6 144.0(4) . . ? C3 Mo1 C8 144.2(5) . . ? C7 Mo1 C8 77.7(6) . . ? C5 Mo1 C8 142.2(5) . . ? C2 Mo1 C8 73.7(6) . . ? C4 Mo1 C8 111.9(5) . . ? C1 Mo1 C8 78.2(5) . . ? C6 Mo1 C8 73.9(4) . . ? C1 N1 Sm1 172.7(9) . . ? C6 N6 Sm1 173.8(9) . 1_545 ? C11 N9 C13 120.2(14) . . ? C11 N9 C12 119.6(12) . . ? C13 N9 C12 120.0(14) . . ? C9 N10 C17 118.6(16) . . ? C9 N10 C18 120.2(16) . . ? C17 N10 C18 120.1(15) . . ? C23 N11 C25 111(2) . . ? C23 N11 C26 132(2) . . ? C25 N11 C26 111(2) . . ? C21 N12 C24 121(2) . . ? C21 N12 C22 123(2) . . ? C24 N12 C22 116(2) . . ? C15 N13 C16 122.6(14) . . ? C15 N13 C14 118.2(17) . . ? C16 N13 C14 119.2(16) . . ? C10 N14 C20 118.9(14) . . ? C10 N14 C19 120.2(13) . . ? C20 N14 C19 120.3(14) . . ? C10 O1 Sm1 132.2(8) . . ? C9 O2 Sm1 134.8(10) . . ? C16 O3 Sm1 138.1(10) . . ? C21 O4 Sm1 143.1(14) . . ? C23 O5 Sm1 150.3(15) . . ? C11 O6 Sm1 137.5(9) . . ? O3 Sm1 O4 77.2(5) . . ? O3 Sm1 O5 140.1(4) . . ? O4 Sm1 O5 73.2(5) . . ? O3 Sm1 O6 109.6(4) . . ? O4 Sm1 O6 145.8(4) . . ? O5 Sm1 O6 82.6(4) . . ? O3 Sm1 O2 79.3(4) . . ? O4 Sm1 O2 73.4(4) . . ? O5 Sm1 O2 115.9(4) . . ? O6 Sm1 O2 140.2(3) . . ? O3 Sm1 O1 74.6(3) . . ? O4 Sm1 O1 139.6(4) . . ? O5 Sm1 O1 143.6(4) . . ? O6 Sm1 O1 72.1(3) . . ? O2 Sm1 O1 73.5(3) . . ? O3 Sm1 N1 144.4(3) . . ? O4 Sm1 N1 114.3(4) . . ? O5 Sm1 N1 73.7(3) . . ? O6 Sm1 N1 80.2(3) . . ? O2 Sm1 N1 72.9(3) . . ? O1 Sm1 N1 76.5(3) . . ? O3 Sm1 N6 70.3(3) . 1_565 ? O4 Sm1 N6 75.7(4) . 1_565 ? O5 Sm1 N6 76.8(4) . 1_565 ? O6 Sm1 N6 75.5(3) . 1_565 ? O2 Sm1 N6 140.6(3) . 1_565 ? O1 Sm1 N6 119.6(3) . 1_565 ? N1 Sm1 N6 143.8(3) . 1_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C3 Mo1 C7 21(14) . . . . ? N2 C3 Mo1 C5 -44(14) . . . . ? N2 C3 Mo1 C2 162(14) . . . . ? N2 C3 Mo1 C4 -124(14) . . . . ? N2 C3 Mo1 C1 85(14) . . . . ? N2 C3 Mo1 C6 -78(14) . . . . ? N2 C3 Mo1 C8 120(14) . . . . ? N8 C7 Mo1 C3 65(82) . . . . ? N8 C7 Mo1 C5 127(82) . . . . ? N8 C7 Mo1 C2 -36(82) . . . . ? N8 C7 Mo1 C4 171(100) . . . . ? N8 C7 Mo1 C1 2(82) . . . . ? N8 C7 Mo1 C6 -155(82) . . . . ? N8 C7 Mo1 C8 -79(82) . . . . ? N5 C5 Mo1 C3 86(34) . . . . ? N5 C5 Mo1 C7 -34(34) . . . . ? N5 C5 Mo1 C2 129(33) . . . . ? N5 C5 Mo1 C4 171(34) . . . . ? N5 C5 Mo1 C1 29(34) . . . . ? N5 C5 Mo1 C6 -115(34) . . . . ? N5 C5 Mo1 C8 -78(34) . . . . ? N3 C2 Mo1 C3 -106(24) . . . . ? N3 C2 Mo1 C7 6(24) . . . . ? N3 C2 Mo1 C5 -147(23) . . . . ? N3 C2 Mo1 C4 170(24) . . . . ? N3 C2 Mo1 C1 -32(24) . . . . ? N3 C2 Mo1 C6 112(24) . . . . ? N3 C2 Mo1 C8 50(24) . . . . ? N4 C4 Mo1 C3 111(52) . . . . ? N4 C4 Mo1 C7 -4(52) . . . . ? N4 C4 Mo1 C5 38(52) . . . . ? N4 C4 Mo1 C2 -167(52) . . . . ? N4 C4 Mo1 C1 158(52) . . . . ? N4 C4 Mo1 C6 -40(52) . . . . ? N4 C4 Mo1 C8 -104(52) . . . . ? N1 C1 Mo1 C3 156(89) . . . . ? N1 C1 Mo1 C7 -84(89) . . . . ? N1 C1 Mo1 C5 -147(89) . . . . ? N1 C1 Mo1 C2 72(89) . . . . ? N1 C1 Mo1 C4 107(89) . . . . ? N1 C1 Mo1 C6 -43(89) . . . . ? N1 C1 Mo1 C8 -4(89) . . . . ? N6 C6 Mo1 C3 -3(16) . . . . ? N6 C6 Mo1 C7 -113(16) . . . . ? N6 C6 Mo1 C5 -36(16) . . . . ? N6 C6 Mo1 C2 105(16) . . . . ? N6 C6 Mo1 C4 47(16) . . . . ? N6 C6 Mo1 C1 -153(16) . . . . ? N6 C6 Mo1 C8 167(16) . . . . ? N7 C8 Mo1 C3 -118(19) . . . . ? N7 C8 Mo1 C7 -8(19) . . . . ? N7 C8 Mo1 C5 36(19) . . . . ? N7 C8 Mo1 C2 -161(19) . . . . ? N7 C8 Mo1 C4 136(19) . . . . ? N7 C8 Mo1 C1 -84(19) . . . . ? N7 C8 Mo1 C6 73(19) . . . . ? Mo1 C1 N1 Sm1 -26(94) . . . . ? Mo1 C6 N6 Sm1 67(21) . . . 1_545 ? O6 C11 N9 C13 178.4(16) . . . . ? O6 C11 N9 C12 2(2) . . . . ? O2 C9 N10 C17 11(3) . . . . ? O2 C9 N10 C18 178.5(18) . . . . ? O5 C23 N11 C25 178(3) . . . . ? O5 C23 N11 C26 27(5) . . . . ? O4 C21 N12 C24 170(3) . . . . ? O4 C21 N12 C22 -16(4) . . . . ? O3 C16 N13 C15 -5(3) . . . . ? O3 C16 N13 C14 173.7(18) . . . . ? O1 C10 N14 C20 178.1(14) . . . . ? O1 C10 N14 C19 7(2) . . . . ? N14 C10 O1 Sm1 -178.9(10) . . . . ? N10 C9 O2 Sm1 -170.4(14) . . . . ? N13 C16 O3 Sm1 167.7(11) . . . . ? N12 C21 O4 Sm1 160.1(18) . . . . ? N11 C23 O5 Sm1 -171.8(19) . . . . ? N9 C11 O6 Sm1 -173.6(10) . . . . ? C16 O3 Sm1 O4 -105.9(18) . . . . ? C16 O3 Sm1 O5 -148.7(16) . . . . ? C16 O3 Sm1 O6 109.0(17) . . . . ? C16 O3 Sm1 O2 -30.7(17) . . . . ? C16 O3 Sm1 O1 44.9(17) . . . . ? C16 O3 Sm1 N1 8(2) . . . . ? C16 O3 Sm1 N6 174.9(18) . . . 1_565 ? C21 O4 Sm1 O3 -85(3) . . . . ? C21 O4 Sm1 O5 68(3) . . . . ? C21 O4 Sm1 O6 21(3) . . . . ? C21 O4 Sm1 O2 -168(3) . . . . ? C21 O4 Sm1 O1 -132(3) . . . . ? C21 O4 Sm1 N1 130(3) . . . . ? C21 O4 Sm1 N6 -13(3) . . . 1_565 ? C23 O5 Sm1 O3 174(3) . . . . ? C23 O5 Sm1 O4 130(3) . . . . ? C23 O5 Sm1 O6 -75(3) . . . . ? C23 O5 Sm1 O2 68(3) . . . . ? C23 O5 Sm1 O1 -29(4) . . . . ? C23 O5 Sm1 N1 7(3) . . . . ? C23 O5 Sm1 N6 -151(3) . . . 1_565 ? C11 O6 Sm1 O3 88.4(14) . . . . ? C11 O6 Sm1 O4 -7.7(18) . . . . ? C11 O6 Sm1 O5 -52.5(14) . . . . ? C11 O6 Sm1 O2 -174.7(12) . . . . ? C11 O6 Sm1 O1 154.0(14) . . . . ? C11 O6 Sm1 N1 -127.1(14) . . . . ? C11 O6 Sm1 N6 25.8(14) . . . 1_565 ? C9 O2 Sm1 O3 117.4(16) . . . . ? C9 O2 Sm1 O4 -162.9(16) . . . . ? C9 O2 Sm1 O5 -101.6(15) . . . . ? C9 O2 Sm1 O6 9.5(18) . . . . ? C9 O2 Sm1 O1 40.5(15) . . . . ? C9 O2 Sm1 N1 -40.1(15) . . . . ? C9 O2 Sm1 N6 157.3(14) . . . 1_565 ? C10 O1 Sm1 O3 156.6(12) . . . . ? C10 O1 Sm1 O4 -156.3(11) . . . . ? C10 O1 Sm1 O5 -8.7(15) . . . . ? C10 O1 Sm1 O6 39.5(11) . . . . ? C10 O1 Sm1 O2 -120.2(12) . . . . ? C10 O1 Sm1 N1 -44.4(12) . . . . ? C10 O1 Sm1 N6 100.4(12) . . . 1_565 ? C1 N1 Sm1 O3 51(7) . . . . ? C1 N1 Sm1 O4 153(7) . . . . ? C1 N1 Sm1 O5 -144(7) . . . . ? C1 N1 Sm1 O6 -59(7) . . . . ? C1 N1 Sm1 O2 91(7) . . . . ? C1 N1 Sm1 O1 14(7) . . . . ? C1 N1 Sm1 N6 -108(7) . . . 1_565 ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.865 _refine_diff_density_min -1.447 _refine_diff_density_rms 0.186 _database_code_depnum_ccdc_archive 'CCDC 889229' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl1 #TrackingRef 'shelxl-Eu.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H42 Eu Mo N14 O6' _chemical_formula_weight 894.64 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' Eu Eu -0.1578 3.6682 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.500(3) _cell_length_b 11.084(2) _cell_length_c 21.108(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.85(3) _cell_angle_gamma 90.00 _cell_volume 3859.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1795 _exptl_absorpt_coefficient_mu 1.989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6687 _exptl_absorpt_correction_T_max 0.7963 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25543 _diffrn_reflns_av_R_equivalents 0.0913 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6714 _reflns_number_gt 5401 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+10.8731P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6714 _refine_ls_number_parameters 445 _refine_ls_number_restraints 119 _refine_ls_R_factor_all 0.0991 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.1743 _refine_ls_wR_factor_gt 0.1619 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.163 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_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_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 C1 C 0.1404(8) 0.3604(11) 0.3902(6) 0.071(3) Uani 1 1 d . . . C2 C 0.1671(8) 0.2686(10) 0.2803(6) 0.063(3) Uani 1 1 d . . . C3 C 0.1993(9) 0.1732(10) 0.4397(6) 0.074(3) Uani 1 1 d . . . C4 C 0.2412(5) 0.0849(10) 0.3311(4) 0.047(2) Uani 1 1 d . . . C5 C 0.3574(8) 0.1923(10) 0.3978(6) 0.072(4) Uani 1 1 d . . . C6 C 0.3316(7) 0.2684(9) 0.2825(6) 0.057(3) Uani 1 1 d . . . C7 C 0.2941(9) 0.3853(11) 0.4403(6) 0.076(4) Uani 1 1 d . . . C8 C 0.2584(6) 0.4566(9) 0.3269(4) 0.043(2) Uani 1 1 d . . . C9 C 0.3758(7) 0.7122(9) 0.4013(5) 0.056(3) Uani 1 1 d . . . H9 H 0.3422 0.6504 0.4149 0.067 Uiso 1 1 calc R . . C10 C 0.4977(9) 0.8269(16) 0.4120(9) 0.120(6) Uani 1 1 d . . . H10A H 0.5378 0.7934 0.3846 0.180 Uiso 1 1 calc R . . H10B H 0.5241 0.8626 0.4483 0.180 Uiso 1 1 calc R . . H10C H 0.4672 0.8875 0.3896 0.180 Uiso 1 1 calc R . . C11 C 0.4702(11) 0.6573(15) 0.4845(8) 0.127(7) Uani 1 1 d . . . H11A H 0.4417 0.5819 0.4829 0.191 Uiso 1 1 calc R . . H11B H 0.4592 0.6972 0.5239 0.191 Uiso 1 1 calc R . . H11C H 0.5274 0.6428 0.4815 0.191 Uiso 1 1 calc R . . C12 C 0.1429(11) 0.8139(16) 0.4121(7) 0.133(4) Uani 1 1 d DU . . H12 H 0.1570 0.8939 0.4195 0.160 Uiso 1 1 calc R . . C13 C 0.0658(16) 0.860(2) 0.4863(12) 0.205(9) Uani 1 1 d DU . . H13A H 0.0218 0.8348 0.5125 0.307 Uiso 1 1 calc R . . H13B H 0.0475 0.9218 0.4578 0.307 Uiso 1 1 calc R . . H13C H 0.1092 0.8903 0.5125 0.307 Uiso 1 1 calc R . . C14 C 0.0253(14) 0.693(2) 0.4337(14) 0.215(9) Uani 1 1 d DU . . H14A H -0.0071 0.7381 0.4039 0.322 Uiso 1 1 calc R . . H14B H -0.0061 0.6752 0.4705 0.322 Uiso 1 1 calc R . . H14C H 0.0426 0.6191 0.4144 0.322 Uiso 1 1 calc R . . C15 C 0.0835(9) 0.6090(15) 0.2510(8) 0.098(5) Uani 1 1 d . . . H15 H 0.0888 0.5727 0.2906 0.117 Uiso 1 1 calc R . . C16 C 0.0119(15) 0.608(3) 0.1542(10) 0.216(14) Uani 1 1 d . . . H16A H 0.0591 0.6462 0.1374 0.324 Uiso 1 1 calc R . . H16B H -0.0312 0.6656 0.1572 0.324 Uiso 1 1 calc R . . H16C H -0.0047 0.5431 0.1267 0.324 Uiso 1 1 calc R . . C17 C -0.0233(9) 0.4650(16) 0.2349(13) 0.182(12) Uani 1 1 d . . . H17A H -0.0126 0.4461 0.2787 0.273 Uiso 1 1 calc R . . H17B H -0.0142 0.3947 0.2095 0.273 Uiso 1 1 calc R . . H17C H -0.0787 0.4905 0.2298 0.273 Uiso 1 1 calc R . . C18 C 0.3038(10) 0.6629(16) 0.1359(9) 0.107(5) Uani 1 1 d . . . H18 H 0.3181 0.7387 0.1208 0.129 Uiso 1 1 calc R . . C19 C 0.3347(17) 0.585(3) 0.0313(11) 0.207(12) Uani 1 1 d . . . H19A H 0.3295 0.6673 0.0175 0.311 Uiso 1 1 calc R . . H19B H 0.3033 0.5337 0.0038 0.311 Uiso 1 1 calc R . . H19C H 0.3907 0.5615 0.0302 0.311 Uiso 1 1 calc R . . C20 C 0.2810(15) 0.4587(15) 0.1125(9) 0.167(9) Uani 1 1 d D . . H20A H 0.2831 0.4508 0.1578 0.251 Uiso 1 1 calc R . . H20B H 0.3165 0.4004 0.0938 0.251 Uiso 1 1 calc R . . H20C H 0.2265 0.4452 0.0975 0.251 Uiso 1 1 calc R . . C21 C 0.1547(15) 0.961(2) 0.0721(11) 0.179(7) Uani 1 1 d U . . H21A H 0.1967 0.9336 0.0446 0.269 Uiso 1 1 calc R . . H21B H 0.1140 1.0028 0.0476 0.269 Uiso 1 1 calc R . . H21C H 0.1307 0.8933 0.0929 0.269 Uiso 1 1 calc R . . C22 C 0.2151(11) 0.9890(19) 0.1716(9) 0.120(5) Uani 1 1 d U . . H22 H 0.2514 1.0312 0.1974 0.144 Uiso 1 1 calc R . . C23 C 0.2234(13) 1.167(2) 0.1059(10) 0.153(7) Uani 1 1 d U . . H23A H 0.1865 1.2277 0.1199 0.229 Uiso 1 1 calc R . . H23B H 0.2299 1.1731 0.0609 0.229 Uiso 1 1 calc R . . H23C H 0.2749 1.1773 0.1268 0.229 Uiso 1 1 calc R . . C24 C 0.4895(9) 0.9533(17) 0.1604(7) 0.111(6) Uani 1 1 d . . . H24A H 0.5467 0.9525 0.1528 0.167 Uiso 1 1 calc R . . H24B H 0.4636 1.0100 0.1322 0.167 Uiso 1 1 calc R . . H24C H 0.4676 0.8742 0.1529 0.167 Uiso 1 1 calc R . . C25 C 0.5317(8) 1.0702(14) 0.2544(8) 0.104(5) Uani 1 1 d . . . H25A H 0.5167 1.0833 0.2977 0.156 Uiso 1 1 calc R . . H25B H 0.5308 1.1456 0.2321 0.156 Uiso 1 1 calc R . . H25C H 0.5853 1.0365 0.2533 0.156 Uiso 1 1 calc R . . C26 C 0.4138(6) 0.9444(9) 0.2552(5) 0.058(3) Uani 1 1 d . . . H26 H 0.4059 0.9699 0.2966 0.069 Uiso 1 1 calc R . . Eu1 Eu 0.24870(3) 0.77477(4) 0.27542(2) 0.03861(18) Uani 1 1 d . . . Mo1 Mo 0.24925(5) 0.27358(7) 0.36089(4) 0.0437(2) Uani 1 1 d . . . N1 N 0.2623(4) 0.5544(7) 0.3106(4) 0.0451(18) Uani 1 1 d . . . N2 N 0.3732(7) 0.2667(10) 0.2406(6) 0.087(3) Uani 1 1 d . . . N3 N 0.1264(7) 0.2671(11) 0.2362(5) 0.092(4) Uani 1 1 d . . . N4 N 0.2387(4) -0.0139(7) 0.3164(4) 0.048(2) Uani 1 1 d . . . N5 N 0.1720(9) 0.1193(11) 0.4782(5) 0.111(5) Uani 1 1 d . . . N6 N 0.4156(8) 0.1451(11) 0.4145(6) 0.101(4) Uani 1 1 d . . . N7 N 0.3198(8) 0.4441(11) 0.4777(5) 0.103(4) Uani 1 1 d . . . N8 N 0.0826(8) 0.4050(12) 0.4049(6) 0.107(4) Uani 1 1 d . . . N9 N 0.4437(6) 0.7326(9) 0.4325(5) 0.077(3) Uani 1 1 d . . . N10 N 0.3055(8) 0.5743(13) 0.0956(6) 0.100(4) Uani 1 1 d D . . N11 N 0.0934(11) 0.7612(16) 0.4516(8) 0.144(4) Uani 1 1 d DU . . N12 N 0.4753(5) 0.9881(8) 0.2249(5) 0.064(2) Uani 1 1 d . . . N13 N 0.0304(6) 0.5614(10) 0.2151(6) 0.085(3) Uani 1 1 d . . . N14 N 0.1908(9) 1.0464(14) 0.1214(7) 0.119(4) Uani 1 1 d U . . O1 O 0.3546(4) 0.7722(6) 0.3543(4) 0.0584(18) Uani 1 1 d . . . O2 O 0.1704(6) 0.7649(8) 0.3675(5) 0.090(3) Uani 1 1 d DU . . O3 O 0.1255(5) 0.6879(8) 0.2434(6) 0.102(4) Uani 1 1 d . . . O4 O 0.2864(6) 0.6569(8) 0.1886(4) 0.082(3) Uani 1 1 d . . . O5 O 0.1984(5) 0.8917(7) 0.1897(4) 0.073(2) Uani 1 1 d . . . O6 O 0.3652(4) 0.8709(7) 0.2322(3) 0.063(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.074(8) 0.067(8) 0.072(8) 0.002(6) 0.033(6) 0.004(6) C2 0.093(8) 0.039(6) 0.057(7) -0.002(5) -0.004(6) 0.023(6) C3 0.128(11) 0.033(6) 0.062(8) -0.002(6) 0.014(7) -0.017(7) C4 0.046(5) 0.052(7) 0.042(5) 0.008(5) -0.001(4) -0.008(4) C5 0.094(9) 0.031(6) 0.090(9) 0.001(6) -0.033(7) 0.001(6) C6 0.067(7) 0.038(6) 0.067(7) 0.009(5) 0.011(6) 0.009(5) C7 0.130(11) 0.042(7) 0.055(7) 0.001(6) -0.008(7) -0.011(7) C8 0.061(6) 0.023(5) 0.046(6) -0.004(4) 0.001(4) 0.006(4) C9 0.068(7) 0.035(6) 0.065(7) -0.004(5) -0.017(5) 0.007(5) C10 0.089(10) 0.129(14) 0.139(15) 0.021(12) -0.038(10) -0.031(10) C11 0.142(14) 0.091(12) 0.146(15) 0.015(11) -0.087(12) 0.004(10) C12 0.134(6) 0.132(6) 0.134(6) 0.001(5) 0.024(5) -0.008(5) C13 0.208(10) 0.199(10) 0.207(10) 0.000(7) 0.007(7) 0.004(7) C14 0.213(10) 0.215(11) 0.216(11) -0.001(7) 0.008(7) -0.004(7) C15 0.084(10) 0.101(12) 0.108(12) 0.015(10) -0.022(9) -0.018(9) C16 0.18(2) 0.35(4) 0.113(17) 0.02(2) -0.049(16) 0.01(2) C17 0.065(10) 0.099(14) 0.38(4) 0.069(19) -0.010(14) -0.024(9) C18 0.132(14) 0.080(11) 0.110(14) -0.007(11) 0.002(11) -0.024(10) C19 0.27(3) 0.21(3) 0.14(2) -0.07(2) 0.02(2) -0.03(2) C20 0.27(3) 0.096(16) 0.131(17) -0.007(14) -0.035(17) 0.011(17) C21 0.187(10) 0.175(11) 0.176(10) 0.008(8) -0.008(8) -0.002(8) C22 0.134(7) 0.116(8) 0.111(7) 0.009(7) -0.012(6) 0.000(7) C23 0.166(10) 0.142(10) 0.151(10) 0.007(8) 0.004(8) -0.013(8) C24 0.090(10) 0.159(17) 0.086(11) -0.021(10) 0.039(8) -0.022(10) C25 0.075(9) 0.092(11) 0.145(14) -0.015(10) 0.016(9) -0.039(8) C26 0.054(6) 0.050(7) 0.070(7) 0.008(6) 0.016(5) -0.014(5) Eu1 0.0419(3) 0.0243(3) 0.0496(3) 0.0005(2) 0.00089(19) -0.00312(19) Mo1 0.0666(5) 0.0222(4) 0.0422(5) 0.0000(4) 0.0008(4) -0.0009(4) N1 0.053(5) 0.031(5) 0.051(5) 0.001(4) 0.003(4) 0.005(3) N2 0.089(8) 0.074(8) 0.098(9) 0.008(6) 0.031(7) 0.017(6) N3 0.106(9) 0.101(9) 0.069(7) -0.023(6) -0.030(6) 0.037(7) N4 0.055(5) 0.017(4) 0.072(6) -0.004(4) 0.003(4) -0.004(3) N5 0.196(14) 0.076(8) 0.062(7) 0.018(7) 0.039(8) -0.012(8) N6 0.110(9) 0.082(9) 0.111(10) 0.008(7) -0.041(8) 0.006(7) N7 0.170(12) 0.071(8) 0.068(7) -0.026(6) -0.017(7) -0.040(8) N8 0.096(9) 0.107(10) 0.119(10) 0.004(8) 0.051(8) 0.015(7) N9 0.075(7) 0.062(6) 0.093(8) 0.000(6) -0.034(6) -0.001(5) N10 0.129(10) 0.100(10) 0.069(8) -0.042(8) 0.008(7) 0.007(8) N11 0.145(7) 0.148(7) 0.141(7) -0.005(6) 0.042(6) -0.028(6) N12 0.048(5) 0.051(6) 0.094(7) 0.005(5) 0.017(5) -0.007(4) N13 0.048(5) 0.071(7) 0.135(10) -0.015(7) -0.035(6) -0.007(5) N14 0.140(6) 0.110(7) 0.106(6) 0.015(6) -0.021(6) -0.012(6) O1 0.058(4) 0.048(4) 0.069(5) 0.005(4) -0.015(4) -0.008(3) O2 0.099(5) 0.074(5) 0.100(5) -0.008(4) 0.047(4) 0.001(4) O3 0.071(6) 0.064(6) 0.170(10) 0.033(6) -0.041(6) -0.034(5) O4 0.147(8) 0.057(6) 0.043(4) -0.005(4) 0.016(5) -0.004(5) O5 0.091(6) 0.045(5) 0.083(6) 0.018(4) -0.020(4) -0.013(4) O6 0.057(4) 0.062(5) 0.070(5) -0.008(4) 0.021(4) -0.019(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N8 1.123(14) . ? C1 Mo1 2.136(12) . ? C2 N3 1.141(14) . ? C2 Mo1 2.160(12) . ? C3 N5 1.109(14) . ? C3 Mo1 2.174(13) . ? C4 N4 1.138(12) . ? C4 Mo1 2.188(11) . ? C5 N6 1.145(14) . ? C5 Mo1 2.136(13) . ? C6 N2 1.127(14) . ? C6 Mo1 2.157(12) . ? C7 N7 1.104(14) . ? C7 Mo1 2.203(12) . ? C8 N1 1.139(11) . ? C8 Mo1 2.158(10) . ? C9 O1 1.241(12) . ? C9 N9 1.311(13) . ? C9 H9 0.9300 . ? C10 N9 1.445(17) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N9 1.441(17) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 O2 1.184(9) . ? C12 N11 1.313(9) . ? C12 H12 0.9300 . ? C13 N11 1.395(10) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N11 1.401(10) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 O3 1.128(15) . ? C15 N13 1.266(16) . ? C15 H15 0.9300 . ? C16 N13 1.41(2) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N13 1.454(18) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 O4 1.155(18) . ? C18 N10 1.300(19) . ? C18 H18 0.9300 . ? C19 N10 1.45(2) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N10 1.392(9) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N14 1.52(2) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 O5 1.18(2) . ? C22 N14 1.29(2) . ? C22 H22 0.9300 . ? C23 N14 1.47(2) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N12 1.439(15) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N12 1.436(15) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O6 1.238(12) . ? C26 N12 1.301(12) . ? C26 H26 0.9300 . ? Eu1 O3 2.340(8) . ? Eu1 O4 2.341(8) . ? Eu1 O2 2.351(9) . ? Eu1 O5 2.366(8) . ? Eu1 O6 2.390(6) . ? Eu1 O1 2.395(7) . ? Eu1 N4 2.503(8) 1_565 ? Eu1 N1 2.562(8) . ? N4 Eu1 2.503(8) 1_545 ? 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 N8 C1 Mo1 179.0(14) . . ? N3 C2 Mo1 177.2(13) . . ? N5 C3 Mo1 177.1(12) . . ? N4 C4 Mo1 178.4(9) . . ? N6 C5 Mo1 176.2(12) . . ? N2 C6 Mo1 178.3(11) . . ? N7 C7 Mo1 175.8(13) . . ? N1 C8 Mo1 178.0(9) . . ? O1 C9 N9 122.6(11) . . ? O1 C9 H9 118.7 . . ? N9 C9 H9 118.7 . . ? N9 C10 H10A 109.5 . . ? N9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N9 C11 H11A 109.5 . . ? N9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O2 C12 N11 123.5(17) . . ? O2 C12 H12 118.3 . . ? N11 C12 H12 118.3 . . ? N11 C13 H13A 109.5 . . ? N11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N11 C14 H14A 109.5 . . ? N11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 N13 131.2(16) . . ? O3 C15 H15 114.4 . . ? N13 C15 H15 114.4 . . ? N13 C16 H16A 109.5 . . ? N13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N13 C17 H17A 109.5 . . ? N13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 N10 126.5(17) . . ? O4 C18 H18 116.7 . . ? N10 C18 H18 116.7 . . ? N10 C19 H19A 109.5 . . ? N10 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N10 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N10 C20 H20A 109.5 . . ? N10 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N10 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N14 C21 H21A 109.5 . . ? N14 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N14 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O5 C22 N14 130.1(19) . . ? O5 C22 H22 114.9 . . ? N14 C22 H22 114.9 . . ? N14 C23 H23A 109.5 . . ? N14 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N14 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N12 C24 H24A 109.5 . . ? N12 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N12 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N12 C25 H25A 109.5 . . ? N12 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N12 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O6 C26 N12 124.0(11) . . ? O6 C26 H26 118.0 . . ? N12 C26 H26 118.0 . . ? O3 Eu1 O4 77.5(4) . . ? O3 Eu1 O2 74.6(4) . . ? O4 Eu1 O2 140.9(3) . . ? O3 Eu1 O5 73.2(3) . . ? O4 Eu1 O5 78.6(3) . . ? O2 Eu1 O5 117.8(3) . . ? O3 Eu1 O6 140.6(3) . . ? O4 Eu1 O6 74.1(3) . . ? O2 Eu1 O6 142.3(3) . . ? O5 Eu1 O6 74.9(3) . . ? O3 Eu1 O1 144.8(3) . . ? O4 Eu1 O1 109.7(3) . . ? O2 Eu1 O1 80.2(3) . . ? O5 Eu1 O1 141.4(2) . . ? O6 Eu1 O1 71.8(3) . . ? O3 Eu1 N4 115.0(3) . 1_565 ? O4 Eu1 N4 144.3(3) . 1_565 ? O2 Eu1 N4 73.6(3) . 1_565 ? O5 Eu1 N4 74.2(3) . 1_565 ? O6 Eu1 N4 76.8(2) . 1_565 ? O1 Eu1 N4 79.8(2) . 1_565 ? O3 Eu1 N1 76.3(3) . . ? O4 Eu1 N1 70.8(3) . . ? O2 Eu1 N1 76.3(3) . . ? O5 Eu1 N1 140.5(3) . . ? O6 Eu1 N1 117.9(3) . . ? O1 Eu1 N1 74.2(2) . . ? N4 Eu1 N1 143.0(3) 1_565 . ? C1 Mo1 C5 141.8(5) . . ? C1 Mo1 C6 140.9(4) . . ? C5 Mo1 C6 74.7(5) . . ? C1 Mo1 C8 74.7(4) . . ? C5 Mo1 C8 117.1(4) . . ? C6 Mo1 C8 73.9(4) . . ? C1 Mo1 C2 73.7(5) . . ? C5 Mo1 C2 141.9(4) . . ? C6 Mo1 C2 77.9(5) . . ? C8 Mo1 C2 79.0(4) . . ? C1 Mo1 C3 71.3(5) . . ? C5 Mo1 C3 80.2(5) . . ? C6 Mo1 C3 145.4(4) . . ? C8 Mo1 C3 139.9(4) . . ? C2 Mo1 C3 110.5(5) . . ? C1 Mo1 C4 117.8(4) . . ? C5 Mo1 C4 75.4(4) . . ? C6 Mo1 C4 77.9(4) . . ? C8 Mo1 C4 143.9(3) . . ? C2 Mo1 C4 73.4(4) . . ? C3 Mo1 C4 73.0(4) . . ? C1 Mo1 C7 78.5(5) . . ? C5 Mo1 C7 72.0(5) . . ? C6 Mo1 C7 113.0(5) . . ? C8 Mo1 C7 72.5(4) . . ? C2 Mo1 C7 144.4(4) . . ? C3 Mo1 C7 80.3(4) . . ? C4 Mo1 C7 140.7(4) . . ? C8 N1 Eu1 171.7(7) . . ? C4 N4 Eu1 172.6(8) . 1_545 ? C9 N9 C11 122.1(12) . . ? C9 N9 C10 120.0(11) . . ? C11 N9 C10 117.8(11) . . ? C18 N10 C20 121.2(16) . . ? C18 N10 C19 124.1(17) . . ? C20 N10 C19 114.7(16) . . ? C12 N11 C13 101.4(17) . . ? C12 N11 C14 125(2) . . ? C13 N11 C14 107(2) . . ? C26 N12 C25 121.9(11) . . ? C26 N12 C24 120.3(11) . . ? C25 N12 C24 117.8(11) . . ? C15 N13 C16 122.1(17) . . ? C15 N13 C17 123.6(16) . . ? C16 N13 C17 113.9(16) . . ? C22 N14 C23 121.0(17) . . ? C22 N14 C21 111.6(17) . . ? C23 N14 C21 123.3(16) . . ? C9 O1 Eu1 139.2(7) . . ? C12 O2 Eu1 149.1(11) . . ? C15 O3 Eu1 144.2(11) . . ? C18 O4 Eu1 142.6(11) . . ? C22 O5 Eu1 131.9(11) . . ? C26 O6 Eu1 131.6(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 C1 Mo1 C5 -136(75) . . . . ? N8 C1 Mo1 C6 72(75) . . . . ? N8 C1 Mo1 C8 109(75) . . . . ? N8 C1 Mo1 C2 26(75) . . . . ? N8 C1 Mo1 C3 -93(75) . . . . ? N8 C1 Mo1 C4 -34(75) . . . . ? N8 C1 Mo1 C7 -176(100) . . . . ? N6 C5 Mo1 C1 155(19) . . . . ? N6 C5 Mo1 C6 -43(19) . . . . ? N6 C5 Mo1 C8 -106(19) . . . . ? N6 C5 Mo1 C2 2(20) . . . . ? N6 C5 Mo1 C3 113(19) . . . . ? N6 C5 Mo1 C4 38(19) . . . . ? N6 C5 Mo1 C7 -164(19) . . . . ? N2 C6 Mo1 C1 -22(39) . . . . ? N2 C6 Mo1 C5 175(100) . . . . ? N2 C6 Mo1 C8 -60(39) . . . . ? N2 C6 Mo1 C2 22(39) . . . . ? N2 C6 Mo1 C3 130(39) . . . . ? N2 C6 Mo1 C4 97(39) . . . . ? N2 C6 Mo1 C7 -123(39) . . . . ? N1 C8 Mo1 C1 38(26) . . . . ? N1 C8 Mo1 C5 -102(26) . . . . ? N1 C8 Mo1 C6 -165(26) . . . . ? N1 C8 Mo1 C2 114(26) . . . . ? N1 C8 Mo1 C3 6(26) . . . . ? N1 C8 Mo1 C4 155(26) . . . . ? N1 C8 Mo1 C7 -44(26) . . . . ? N3 C2 Mo1 C1 139(21) . . . . ? N3 C2 Mo1 C5 -58(21) . . . . ? N3 C2 Mo1 C6 -13(21) . . . . ? N3 C2 Mo1 C8 62(21) . . . . ? N3 C2 Mo1 C3 -158(21) . . . . ? N3 C2 Mo1 C4 -94(21) . . . . ? N3 C2 Mo1 C7 99(21) . . . . ? N5 C3 Mo1 C1 88(28) . . . . ? N5 C3 Mo1 C5 -117(28) . . . . ? N5 C3 Mo1 C6 -74(28) . . . . ? N5 C3 Mo1 C8 122(28) . . . . ? N5 C3 Mo1 C2 25(28) . . . . ? N5 C3 Mo1 C4 -40(28) . . . . ? N5 C3 Mo1 C7 169(28) . . . . ? N4 C4 Mo1 C1 -137(33) . . . . ? N4 C4 Mo1 C5 5(33) . . . . ? N4 C4 Mo1 C6 82(33) . . . . ? N4 C4 Mo1 C8 121(33) . . . . ? N4 C4 Mo1 C2 163(33) . . . . ? N4 C4 Mo1 C3 -79(33) . . . . ? N4 C4 Mo1 C7 -30(34) . . . . ? N7 C7 Mo1 C1 -125(18) . . . . ? N7 C7 Mo1 C5 79(18) . . . . ? N7 C7 Mo1 C6 15(18) . . . . ? N7 C7 Mo1 C8 -48(18) . . . . ? N7 C7 Mo1 C2 -86(18) . . . . ? N7 C7 Mo1 C3 162(18) . . . . ? N7 C7 Mo1 C4 114(18) . . . . ? Mo1 C8 N1 Eu1 -59(29) . . . . ? O3 Eu1 N1 C8 -29(5) . . . . ? O4 Eu1 N1 C8 -111(5) . . . . ? O2 Eu1 N1 C8 48(5) . . . . ? O5 Eu1 N1 C8 -70(5) . . . . ? O6 Eu1 N1 C8 -170(5) . . . . ? O1 Eu1 N1 C8 131(5) . . . . ? N4 Eu1 N1 C8 84(5) 1_565 . . . ? Mo1 C4 N4 Eu1 -70(36) . . . 1_545 ? O1 C9 N9 C11 -175.9(13) . . . . ? O1 C9 N9 C10 -0.8(19) . . . . ? O4 C18 N10 C20 3(3) . . . . ? O4 C18 N10 C19 -174(2) . . . . ? O2 C12 N11 C13 -168(2) . . . . ? O2 C12 N11 C14 -48(4) . . . . ? O6 C26 N12 C25 -177.9(12) . . . . ? O6 C26 N12 C24 1.1(18) . . . . ? O3 C15 N13 C16 -2(3) . . . . ? O3 C15 N13 C17 -174.8(19) . . . . ? O5 C22 N14 C23 -176.5(19) . . . . ? O5 C22 N14 C21 -18(3) . . . . ? N9 C9 O1 Eu1 174.9(8) . . . . ? O3 Eu1 O1 C9 6.7(14) . . . . ? O4 Eu1 O1 C9 -89.7(11) . . . . ? O2 Eu1 O1 C9 51.1(11) . . . . ? O5 Eu1 O1 C9 173.9(10) . . . . ? O6 Eu1 O1 C9 -154.6(11) . . . . ? N4 Eu1 O1 C9 126.0(11) 1_565 . . . ? N1 Eu1 O1 C9 -27.3(11) . . . . ? N11 C12 O2 Eu1 175.4(14) . . . . ? O3 Eu1 O2 C12 -128(2) . . . . ? O4 Eu1 O2 C12 -174(2) . . . . ? O5 Eu1 O2 C12 -67(3) . . . . ? O6 Eu1 O2 C12 35(3) . . . . ? O1 Eu1 O2 C12 77(2) . . . . ? N4 Eu1 O2 C12 -5(2) 1_565 . . . ? N1 Eu1 O2 C12 153(3) . . . . ? N13 C15 O3 Eu1 -155.6(14) . . . . ? O4 Eu1 O3 C15 92(2) . . . . ? O2 Eu1 O3 C15 -60(2) . . . . ? O5 Eu1 O3 C15 174(2) . . . . ? O6 Eu1 O3 C15 137(2) . . . . ? O1 Eu1 O3 C15 -14(3) . . . . ? N4 Eu1 O3 C15 -123(2) 1_565 . . . ? N1 Eu1 O3 C15 19(2) . . . . ? N10 C18 O4 Eu1 -164.0(11) . . . . ? O3 Eu1 O4 C18 104.2(18) . . . . ? O2 Eu1 O4 C18 149.4(17) . . . . ? O5 Eu1 O4 C18 29.0(18) . . . . ? O6 Eu1 O4 C18 -48.3(18) . . . . ? O1 Eu1 O4 C18 -111.8(18) . . . . ? N4 Eu1 O4 C18 -12(2) 1_565 . . . ? N1 Eu1 O4 C18 -176.2(19) . . . . ? N14 C22 O5 Eu1 173.7(14) . . . . ? O3 Eu1 O5 C22 163.4(16) . . . . ? O4 Eu1 O5 C22 -116.3(15) . . . . ? O2 Eu1 O5 C22 101.7(15) . . . . ? O6 Eu1 O5 C22 -39.9(15) . . . . ? O1 Eu1 O5 C22 -9.0(17) . . . . ? N4 Eu1 O5 C22 40.4(15) 1_565 . . . ? N1 Eu1 O5 C22 -155.7(14) . . . . ? N12 C26 O6 Eu1 179.6(8) . . . . ? O3 Eu1 O6 C26 154.0(9) . . . . ? O4 Eu1 O6 C26 -160.5(10) . . . . ? O2 Eu1 O6 C26 1.2(12) . . . . ? O5 Eu1 O6 C26 117.3(10) . . . . ? O1 Eu1 O6 C26 -42.9(9) . . . . ? N4 Eu1 O6 C26 40.4(9) 1_565 . . . ? N1 Eu1 O6 C26 -103.1(10) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.389 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.140 _database_code_depnum_ccdc_archive 'CCDC 881382' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl #TrackingRef 'shelxl-Gd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H42 Gd Mo N14 O6' _chemical_formula_weight 899.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.426(3) _cell_length_b 11.051(2) _cell_length_c 21.097(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.17(3) _cell_angle_gamma 90.00 _cell_volume 3828.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1799 _exptl_absorpt_coefficient_mu 2.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6552 _exptl_absorpt_correction_T_max 0.7868 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30558 _diffrn_reflns_av_R_equivalents 0.0875 _diffrn_reflns_av_sigmaI/netI 0.0720 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6738 _reflns_number_gt 5273 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+2.7249P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6738 _refine_ls_number_parameters 445 _refine_ls_number_restraints 76 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1713 _refine_ls_wR_factor_gt 0.1567 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.074 _refine_ls_shift/su_mean 0.007 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 C1 C 0.2416(5) -0.4132(8) 0.8320(3) 0.0421(18) Uani 1 1 d . . . C2 C 0.1670(6) -0.2296(8) 0.7807(5) 0.056(2) Uani 1 1 d . . . C3 C 0.1384(6) -0.1409(8) 0.8906(4) 0.060(2) Uani 1 1 d . . . C4 C 0.2587(4) -0.0434(7) 0.8269(3) 0.0384(17) Uani 1 1 d . . . C5 C 0.3307(6) -0.2325(8) 0.7819(5) 0.054(2) Uani 1 1 d . . . C6 C 0.2939(6) -0.1158(9) 0.9381(4) 0.063(2) Uani 1 1 d . . . C7 C 0.3584(6) -0.3125(9) 0.8985(5) 0.063(2) Uani 1 1 d . . . C8 C 0.2010(7) -0.3277(9) 0.9393(4) 0.067(3) Uani 1 1 d . . . C9 C 0.1401(11) 0.2802(17) 0.9054(9) 0.143(4) Uani 1 1 d U . . H9 H 0.1593 0.3573 0.9149 0.172 Uiso 1 1 calc R . . C10 C 0.0283(13) 0.190(2) 0.9424(13) 0.248(9) Uani 1 1 d DU . . H10A H -0.0204 0.2362 0.9351 0.372 Uiso 1 1 calc R . . H10B H 0.0222 0.1404 0.9794 0.372 Uiso 1 1 calc R . . H10C H 0.0378 0.1390 0.9064 0.372 Uiso 1 1 calc R . . C11 C 0.0534(14) 0.3579(18) 0.9837(11) 0.224(8) Uani 1 1 d DU . . H11A H 0.0127 0.3933 0.9562 0.335 Uiso 1 1 calc R . . H11B H 0.0915 0.4191 0.9970 0.335 Uiso 1 1 calc R . . H11C H 0.0279 0.3239 1.0201 0.335 Uiso 1 1 calc R . . C12 C 0.0174(14) 0.097(3) 0.6529(7) 0.258(15) Uani 1 1 d D . . H12A H -0.0384 0.1211 0.6470 0.387 Uiso 1 1 calc R . . H12B H 0.0292 0.0315 0.6246 0.387 Uiso 1 1 calc R . . H12C H 0.0524 0.1642 0.6440 0.387 Uiso 1 1 calc R . . C13 C -0.0232(9) -0.0298(17) 0.7384(10) 0.198(11) Uani 1 1 d . . . H13A H -0.0271 -0.0218 0.7836 0.297 Uiso 1 1 calc R . . H13B H -0.0028 -0.1088 0.7284 0.297 Uiso 1 1 calc R . . H13C H -0.0762 -0.0193 0.7191 0.297 Uiso 1 1 calc R . . C14 C 0.0838(7) 0.1104(13) 0.7505(7) 0.100(4) Uani 1 1 d . . . H14 H 0.0888 0.0742 0.7902 0.120 Uiso 1 1 calc R . . C15 C 0.3776(5) 0.2137(8) 0.9006(4) 0.053(2) Uani 1 1 d . . . H15 H 0.3444 0.1511 0.9143 0.064 Uiso 1 1 calc R . . C16 C 0.4997(7) 0.3290(13) 0.9116(7) 0.115(5) Uani 1 1 d . . . H16A H 0.5234 0.3072 0.8720 0.173 Uiso 1 1 calc R . . H16B H 0.5421 0.3399 0.9431 0.173 Uiso 1 1 calc R . . H16C H 0.4697 0.4030 0.9065 0.173 Uiso 1 1 calc R . . C17 C 0.4719(8) 0.1594(11) 0.9844(6) 0.105(4) Uani 1 1 d . . . H17A H 0.4453 0.0821 0.9823 0.158 Uiso 1 1 calc R . . H17B H 0.4588 0.1990 1.0234 0.158 Uiso 1 1 calc R . . H17C H 0.5298 0.1481 0.9825 0.158 Uiso 1 1 calc R . . C18 C 0.4127(5) 0.4448(8) 0.7551(4) 0.053(2) Uani 1 1 d . . . H18 H 0.4048 0.4726 0.7961 0.063 Uiso 1 1 calc R . . C19 C 0.4879(7) 0.4486(13) 0.6604(5) 0.099(4) Uani 1 1 d . . . H19A H 0.4910 0.3619 0.6589 0.149 Uiso 1 1 calc R . . H19B H 0.5378 0.4826 0.6457 0.149 Uiso 1 1 calc R . . H19C H 0.4434 0.4758 0.6338 0.149 Uiso 1 1 calc R . . C20 C 0.5311(6) 0.5734(11) 0.7553(6) 0.095(4) Uani 1 1 d . . . H20A H 0.5169 0.5829 0.7990 0.143 Uiso 1 1 calc R . . H20B H 0.5270 0.6502 0.7342 0.143 Uiso 1 1 calc R . . H20C H 0.5859 0.5438 0.7529 0.143 Uiso 1 1 calc R . . C21 C 0.2129(10) 0.4888(14) 0.6706(5) 0.121(6) Uani 1 1 d . . . H21 H 0.2489 0.5314 0.6968 0.145 Uiso 1 1 calc R . . C22 C 0.1513(12) 0.474(2) 0.5765(9) 0.194(7) Uani 1 1 d U . . H22A H 0.1908 0.4259 0.5552 0.291 Uiso 1 1 calc R . . H22B H 0.1234 0.5253 0.5463 0.291 Uiso 1 1 calc R . . H22C H 0.1126 0.4224 0.5966 0.291 Uiso 1 1 calc R . . C23 C 0.2142(14) 0.6659(15) 0.6039(8) 0.187(9) Uani 1 1 d . . . H23A H 0.2082 0.7209 0.6387 0.281 Uiso 1 1 calc R . . H23B H 0.1799 0.6915 0.5690 0.281 Uiso 1 1 calc R . . H23C H 0.2699 0.6653 0.5910 0.281 Uiso 1 1 calc R . . C24 C 0.3328(13) 0.087(2) 0.5335(7) 0.216(12) Uani 1 1 d . . . H24A H 0.2929 0.0540 0.5046 0.324 Uiso 1 1 calc R . . H24B H 0.3838 0.0466 0.5283 0.324 Uiso 1 1 calc R . . H24C H 0.3394 0.1720 0.5250 0.324 Uiso 1 1 calc R . . C25 C 0.2819(10) -0.0428(12) 0.6131(7) 0.141(6) Uani 1 1 d D . . H25A H 0.2678 -0.0426 0.6570 0.211 Uiso 1 1 calc R . . H25B H 0.3253 -0.0994 0.6066 0.211 Uiso 1 1 calc R . . H25C H 0.2353 -0.0659 0.5877 0.211 Uiso 1 1 calc R . . C26 C 0.3039(8) 0.1610(12) 0.6370(7) 0.097(4) Uani 1 1 d . . . H26 H 0.3170 0.2376 0.6221 0.117 Uiso 1 1 calc R . . Gd1 Gd 0.24875(2) 0.27444(3) 0.775982(17) 0.03411(17) Uani 1 1 d . . . Mo1 Mo 0.24941(4) -0.22696(6) 0.86115(3) 0.0379(2) Uani 1 1 d . . . N1 N 0.3725(6) -0.2341(7) 0.7401(5) 0.075(3) Uani 1 1 d . . . N2 N 0.1266(6) -0.2326(9) 0.7371(5) 0.091(3) Uani 1 1 d . . . N3 N 0.2392(4) -0.5114(6) 0.8165(3) 0.0472(16) Uani 1 1 d . . . N4 N 0.1708(7) -0.3807(9) 0.9786(4) 0.101(3) Uani 1 1 d . . . N5 N 0.4174(6) -0.3585(9) 0.9151(5) 0.097(3) Uani 1 1 d . . . N6 N 0.3174(7) -0.0558(9) 0.9785(4) 0.093(3) Uani 1 1 d . . . N7 N 0.0806(6) -0.0960(10) 0.9060(5) 0.101(3) Uani 1 1 d . . . N8 N 0.2619(4) 0.0560(6) 0.8114(3) 0.0436(15) Uani 1 1 d . . . N9 N 0.4448(5) 0.2328(7) 0.9317(4) 0.071(2) Uani 1 1 d . . . N10 N 0.4749(4) 0.4865(7) 0.7244(4) 0.061(2) Uani 1 1 d . . . N11 N 0.1911(7) 0.5471(9) 0.6230(4) 0.100(3) Uani 1 1 d U . . N12 N 0.3069(6) 0.0719(9) 0.5956(4) 0.088(3) Uani 1 1 d D . . N13 N 0.0306(5) 0.0595(8) 0.7151(5) 0.079(3) Uani 1 1 d D . . N14 N 0.0940(9) 0.2676(13) 0.9514(7) 0.139(4) Uani 1 1 d DU . . O1 O 0.1261(4) 0.1892(7) 0.7447(4) 0.093(3) Uani 1 1 d . . . O2 O 0.1980(4) 0.3905(6) 0.6904(3) 0.0664(18) Uani 1 1 d . . . O3 O 0.1703(5) 0.2672(7) 0.8666(4) 0.087(2) Uani 1 1 d U . . O4 O 0.3644(3) 0.3716(6) 0.7332(3) 0.0590(16) Uani 1 1 d . . . O5 O 0.3541(3) 0.2725(5) 0.8540(3) 0.0547(16) Uani 1 1 d . . . O6 O 0.2867(4) 0.1549(6) 0.6900(3) 0.0683(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.052(5) 0.029(5) 0.045(4) 0.006(3) 0.005(3) -0.004(4) C2 0.067(6) 0.044(6) 0.056(6) -0.008(4) -0.012(5) 0.010(4) C3 0.075(6) 0.047(6) 0.059(5) 0.003(4) 0.025(5) 0.001(5) C4 0.053(5) 0.019(4) 0.043(4) -0.006(3) 0.001(3) -0.002(3) C5 0.069(6) 0.038(5) 0.055(6) 0.001(4) -0.001(5) 0.021(4) C6 0.099(7) 0.038(6) 0.051(5) -0.002(4) 0.000(5) -0.013(5) C7 0.072(6) 0.045(6) 0.071(6) -0.006(5) -0.026(5) 0.001(5) C8 0.117(8) 0.037(5) 0.047(5) 0.003(4) 0.011(5) -0.005(5) C9 0.139(7) 0.162(7) 0.130(7) 0.003(6) 0.041(6) -0.007(6) C10 0.244(12) 0.245(12) 0.256(12) -0.008(9) 0.017(9) -0.009(9) C11 0.230(11) 0.212(11) 0.229(11) -0.004(9) 0.016(9) -0.004(9) C12 0.22(2) 0.44(5) 0.106(14) 0.01(2) -0.024(15) -0.07(3) C13 0.078(9) 0.129(17) 0.39(3) 0.087(19) -0.031(14) -0.029(10) C14 0.064(7) 0.097(11) 0.138(11) -0.016(8) -0.020(7) -0.014(7) C15 0.058(5) 0.039(5) 0.062(6) -0.004(4) -0.019(4) 0.000(4) C16 0.073(8) 0.112(11) 0.159(13) 0.020(10) -0.046(8) -0.040(8) C17 0.122(10) 0.074(9) 0.117(10) 0.016(7) -0.055(8) 0.011(8) C18 0.039(4) 0.044(6) 0.077(6) 0.010(4) 0.013(4) -0.006(4) C19 0.085(8) 0.133(12) 0.081(8) -0.006(7) 0.036(6) -0.023(8) C20 0.047(6) 0.071(8) 0.169(12) -0.014(8) 0.025(7) -0.023(5) C21 0.210(16) 0.095(11) 0.058(7) 0.008(7) 0.005(8) 0.072(11) C22 0.205(10) 0.188(10) 0.190(10) 0.016(8) -0.011(8) -0.014(8) C23 0.35(3) 0.085(12) 0.127(13) 0.030(10) 0.071(16) -0.037(16) C24 0.30(3) 0.24(3) 0.106(13) -0.049(14) 0.081(15) -0.12(2) C25 0.218(19) 0.080(12) 0.125(12) 0.004(9) 0.010(12) -0.004(12) C26 0.114(10) 0.066(9) 0.113(11) 0.005(8) 0.006(8) -0.033(7) Gd1 0.0367(3) 0.0197(3) 0.0460(3) 0.00051(14) 0.00120(16) -0.00274(14) Mo1 0.0576(5) 0.0184(4) 0.0377(4) -0.0001(2) 0.0006(3) -0.0007(3) N1 0.097(7) 0.055(6) 0.076(6) -0.001(4) 0.031(5) 0.011(4) N2 0.093(7) 0.095(8) 0.082(7) -0.024(5) -0.036(6) 0.028(5) N3 0.058(4) 0.027(4) 0.058(4) -0.002(3) 0.004(3) -0.003(3) N4 0.177(10) 0.067(7) 0.061(5) 0.011(5) 0.031(6) -0.009(7) N5 0.103(7) 0.077(7) 0.107(7) 0.002(6) -0.052(6) 0.008(6) N6 0.152(9) 0.065(6) 0.061(5) -0.010(5) -0.017(5) -0.033(6) N7 0.081(7) 0.105(9) 0.120(8) -0.004(6) 0.042(6) 0.027(6) N8 0.049(4) 0.027(4) 0.055(4) 0.002(3) 0.009(3) -0.002(3) N9 0.071(5) 0.052(5) 0.088(6) -0.001(4) -0.036(5) 0.005(4) N10 0.036(4) 0.051(5) 0.095(5) 0.016(4) 0.014(4) -0.003(3) N11 0.145(7) 0.080(6) 0.073(5) 0.024(5) -0.022(5) -0.008(5) N12 0.111(7) 0.086(8) 0.066(6) -0.038(5) 0.008(5) -0.006(6) N13 0.036(4) 0.073(7) 0.127(8) -0.018(5) -0.007(4) -0.009(4) N14 0.141(6) 0.153(7) 0.127(6) -0.009(5) 0.066(5) -0.032(6) O1 0.063(4) 0.058(5) 0.155(8) 0.033(5) -0.039(4) -0.043(4) O2 0.085(5) 0.042(4) 0.071(4) 0.022(3) -0.017(3) 0.001(3) O3 0.101(5) 0.073(4) 0.089(5) 0.003(3) 0.067(4) 0.004(4) O4 0.052(3) 0.061(4) 0.065(4) 0.002(3) 0.015(3) -0.022(3) O5 0.052(4) 0.049(4) 0.062(4) 0.008(3) -0.019(3) -0.003(3) O6 0.115(5) 0.052(4) 0.039(3) -0.002(3) 0.015(3) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N3 1.135(10) . ? C1 Mo1 2.151(9) . ? C2 N2 1.125(12) . ? C2 Mo1 2.149(10) . ? C3 N7 1.125(11) . ? C3 Mo1 2.160(10) . ? C4 N8 1.148(9) . ? C4 Mo1 2.160(8) . ? C5 N1 1.128(12) . ? C5 Mo1 2.162(10) . ? C6 N6 1.141(11) . ? C6 Mo1 2.152(9) . ? C7 N5 1.143(11) . ? C7 Mo1 2.159(9) . ? C8 N4 1.137(11) . ? C8 Mo1 2.155(9) . ? C9 O3 0.975(17) . ? C9 N14 1.252(19) . ? C9 H9 0.9300 . ? C10 N14 1.389(10) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N14 1.387(10) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N13 1.390(9) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N13 1.420(17) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 O1 1.123(13) . ? C14 N13 1.269(13) . ? C14 H14 0.9300 . ? C15 O5 1.234(10) . ? C15 N9 1.291(11) . ? C15 H15 0.9300 . ? C16 N9 1.462(14) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N9 1.439(13) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 O4 1.218(9) . ? C18 N10 1.304(10) . ? C18 H18 0.9300 . ? C19 N10 1.434(12) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N10 1.474(13) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 O2 1.189(15) . ? C21 N11 1.240(13) . ? C21 H21 0.9300 . ? C22 N11 1.419(19) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 N11 1.427(17) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N12 1.396(16) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N12 1.385(9) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O6 1.159(13) . ? C26 N12 1.319(14) . ? C26 H26 0.9300 . ? Gd1 O1 2.308(6) . ? Gd1 O3 2.329(7) . ? Gd1 O6 2.340(6) . ? Gd1 O2 2.354(6) . ? Gd1 O5 2.363(6) . ? Gd1 O4 2.376(5) . ? Gd1 N3 2.522(7) 1_565 ? Gd1 N8 2.535(7) . ? N3 Gd1 2.522(7) 1_545 ? 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 N3 C1 Mo1 178.6(7) . . ? N2 C2 Mo1 177.1(10) . . ? N7 C3 Mo1 179.9(12) . . ? N8 C4 Mo1 176.7(6) . . ? N1 C5 Mo1 179.0(9) . . ? N6 C6 Mo1 179.3(9) . . ? N5 C7 Mo1 176.5(10) . . ? N4 C8 Mo1 175.6(11) . . ? O3 C9 N14 164(2) . . ? O3 C9 H9 98.1 . . ? N14 C9 H9 98.1 . . ? N14 C10 H10A 109.4 . . ? N14 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N14 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N14 C11 H11A 109.4 . . ? N14 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N14 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N13 C12 H12A 109.5 . . ? N13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N13 C12 H12C 109.4 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N13 C13 H13A 109.5 . . ? N13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N13 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O1 C14 N13 134.4(15) . . ? O1 C14 H14 112.8 . . ? N13 C14 H14 112.8 . . ? O5 C15 N9 124.7(9) . . ? O5 C15 H15 117.7 . . ? N9 C15 H15 117.6 . . ? N9 C16 H16A 109.5 . . ? N9 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N9 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N9 C17 H17A 109.5 . . ? N9 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N9 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 N10 124.0(9) . . ? O4 C18 H18 118.0 . . ? N10 C18 H18 118.0 . . ? N10 C19 H19A 109.5 . . ? N10 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N10 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N10 C20 H20A 109.5 . . ? N10 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N10 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O2 C21 N11 134.5(16) . . ? O2 C21 H21 112.8 . . ? N11 C21 H21 112.8 . . ? N11 C22 H22A 109.4 . . ? N11 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N11 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N11 C23 H23A 109.5 . . ? N11 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N11 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N12 C24 H24A 109.5 . . ? N12 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N12 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N12 C25 H25A 109.5 . . ? N12 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N12 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O6 C26 N12 127.5(12) . . ? O6 C26 H26 116.3 . . ? N12 C26 H26 116.3 . . ? O1 Gd1 O3 74.1(3) . . ? O1 Gd1 O6 78.1(3) . . ? O3 Gd1 O6 141.1(3) . . ? O1 Gd1 O2 73.1(2) . . ? O3 Gd1 O2 117.1(3) . . ? O6 Gd1 O2 78.9(2) . . ? O1 Gd1 O5 144.9(2) . . ? O3 Gd1 O5 80.7(3) . . ? O6 Gd1 O5 109.4(2) . . ? O2 Gd1 O5 141.4(2) . . ? O1 Gd1 O4 140.9(3) . . ? O3 Gd1 O4 142.0(3) . . ? O6 Gd1 O4 74.5(2) . . ? O2 Gd1 O4 74.7(2) . . ? O5 Gd1 O4 71.9(2) . . ? O1 Gd1 N3 114.8(3) . 1_565 ? O3 Gd1 N3 73.4(2) . 1_565 ? O6 Gd1 N3 144.3(2) . 1_565 ? O2 Gd1 N3 74.0(2) . 1_565 ? O5 Gd1 N3 79.8(2) . 1_565 ? O4 Gd1 N3 76.2(2) . 1_565 ? O1 Gd1 N8 76.4(2) . . ? O3 Gd1 N8 76.7(2) . . ? O6 Gd1 N8 70.6(2) . . ? O2 Gd1 N8 140.5(2) . . ? O5 Gd1 N8 74.3(2) . . ? O4 Gd1 N8 118.6(2) . . ? N3 Gd1 N8 143.1(2) 1_565 . ? C2 Mo1 C1 74.2(3) . . ? C2 Mo1 C6 143.4(4) . . ? C1 Mo1 C6 141.2(3) . . ? C2 Mo1 C8 111.2(4) . . ? C1 Mo1 C8 72.8(3) . . ? C6 Mo1 C8 81.0(4) . . ? C2 Mo1 C7 141.8(4) . . ? C1 Mo1 C7 74.3(3) . . ? C6 Mo1 C7 73.0(4) . . ? C8 Mo1 C7 79.1(4) . . ? C2 Mo1 C3 73.2(4) . . ? C1 Mo1 C3 117.2(3) . . ? C6 Mo1 C3 78.9(4) . . ? C8 Mo1 C3 71.3(4) . . ? C7 Mo1 C3 141.9(4) . . ? C2 Mo1 C4 78.3(3) . . ? C1 Mo1 C4 143.8(3) . . ? C6 Mo1 C4 72.0(3) . . ? C8 Mo1 C4 140.4(3) . . ? C7 Mo1 C4 118.0(3) . . ? C3 Mo1 C4 75.4(3) . . ? C2 Mo1 C5 77.2(4) . . ? C1 Mo1 C5 77.6(3) . . ? C6 Mo1 C5 113.2(4) . . ? C8 Mo1 C5 145.1(3) . . ? C7 Mo1 C5 75.4(4) . . ? C3 Mo1 C5 140.7(3) . . ? C4 Mo1 C5 73.7(3) . . ? C1 N3 Gd1 173.6(6) . 1_545 ? C4 N8 Gd1 172.4(6) . . ? C15 N9 C17 123.3(9) . . ? C15 N9 C16 119.9(9) . . ? C17 N9 C16 116.8(9) . . ? C18 N10 C19 119.7(8) . . ? C18 N10 C20 120.1(9) . . ? C19 N10 C20 120.2(8) . . ? C21 N11 C22 112.7(14) . . ? C21 N11 C23 129.4(15) . . ? C22 N11 C23 116.6(13) . . ? C26 N12 C25 119.5(11) . . ? C26 N12 C24 123.2(13) . . ? C25 N12 C24 117.3(12) . . ? C14 N13 C12 121.1(14) . . ? C14 N13 C13 122.0(13) . . ? C12 N13 C13 116.7(14) . . ? C9 N14 C11 127.2(18) . . ? C9 N14 C10 116.2(19) . . ? C11 N14 C10 97.6(18) . . ? C14 O1 Gd1 145.5(9) . . ? C21 O2 Gd1 134.0(9) . . ? C9 O3 Gd1 169.2(14) . . ? C18 O4 Gd1 132.6(6) . . ? C15 O5 Gd1 140.5(6) . . ? C26 O6 Gd1 142.0(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C2 Mo1 C1 -64(18) . . . . ? N2 C2 Mo1 C6 128(18) . . . . ? N2 C2 Mo1 C8 -128(18) . . . . ? N2 C2 Mo1 C7 -28(19) . . . . ? N2 C2 Mo1 C3 171(19) . . . . ? N2 C2 Mo1 C4 92(18) . . . . ? N2 C2 Mo1 C5 17(18) . . . . ? N3 C1 Mo1 C2 123(27) . . . . ? N3 C1 Mo1 C6 -68(27) . . . . ? N3 C1 Mo1 C8 -118(27) . . . . ? N3 C1 Mo1 C7 -35(27) . . . . ? N3 C1 Mo1 C3 -175(100) . . . . ? N3 C1 Mo1 C4 82(27) . . . . ? N3 C1 Mo1 C5 43(27) . . . . ? N6 C6 Mo1 C2 -31(82) . . . . ? N6 C6 Mo1 C1 168(100) . . . . ? N6 C6 Mo1 C8 -144(82) . . . . ? N6 C6 Mo1 C7 134(82) . . . . ? N6 C6 Mo1 C3 -72(82) . . . . ? N6 C6 Mo1 C4 6(82) . . . . ? N6 C6 Mo1 C5 69(82) . . . . ? N4 C8 Mo1 C2 -15(12) . . . . ? N4 C8 Mo1 C1 -79(12) . . . . ? N4 C8 Mo1 C6 129(12) . . . . ? N4 C8 Mo1 C7 -156(12) . . . . ? N4 C8 Mo1 C3 48(12) . . . . ? N4 C8 Mo1 C4 83(12) . . . . ? N4 C8 Mo1 C5 -113(12) . . . . ? N5 C7 Mo1 C2 31(15) . . . . ? N5 C7 Mo1 C1 67(15) . . . . ? N5 C7 Mo1 C6 -134(15) . . . . ? N5 C7 Mo1 C8 142(15) . . . . ? N5 C7 Mo1 C3 -179(100) . . . . ? N5 C7 Mo1 C4 -76(15) . . . . ? N5 C7 Mo1 C5 -14(15) . . . . ? N7 C3 Mo1 C2 -135(100) . . . . ? N7 C3 Mo1 C1 164(100) . . . . ? N7 C3 Mo1 C6 21(100) . . . . ? N7 C3 Mo1 C8 106(100) . . . . ? N7 C3 Mo1 C7 64(100) . . . . ? N7 C3 Mo1 C4 -53(100) . . . . ? N7 C3 Mo1 C5 -92(100) . . . . ? N8 C4 Mo1 C2 114(12) . . . . ? N8 C4 Mo1 C1 155(12) . . . . ? N8 C4 Mo1 C6 -44(12) . . . . ? N8 C4 Mo1 C8 5(12) . . . . ? N8 C4 Mo1 C7 -103(12) . . . . ? N8 C4 Mo1 C3 38(12) . . . . ? N8 C4 Mo1 C5 -166(12) . . . . ? N1 C5 Mo1 C2 46(60) . . . . ? N1 C5 Mo1 C1 123(60) . . . . ? N1 C5 Mo1 C6 -97(60) . . . . ? N1 C5 Mo1 C8 155(59) . . . . ? N1 C5 Mo1 C7 -161(60) . . . . ? N1 C5 Mo1 C3 4(60) . . . . ? N1 C5 Mo1 C4 -35(60) . . . . ? Mo1 C1 N3 Gd1 -23(32) . . . 1_545 ? Mo1 C4 N8 Gd1 -68(14) . . . . ? O1 Gd1 N8 C4 -20(4) . . . . ? O3 Gd1 N8 C4 57(4) . . . . ? O6 Gd1 N8 C4 -101(4) . . . . ? O2 Gd1 N8 C4 -60(5) . . . . ? O5 Gd1 N8 C4 141(4) . . . . ? O4 Gd1 N8 C4 -161(4) . . . . ? N3 Gd1 N8 C4 94(4) 1_565 . . . ? O5 C15 N9 C17 -177.4(11) . . . . ? O5 C15 N9 C16 -0.9(17) . . . . ? O4 C18 N10 C19 1.8(14) . . . . ? O4 C18 N10 C20 -178.9(9) . . . . ? O2 C21 N11 C22 -13(2) . . . . ? O2 C21 N11 C23 -179.2(16) . . . . ? O6 C26 N12 C25 5(2) . . . . ? O6 C26 N12 C24 -176.3(16) . . . . ? O1 C14 N13 C12 3(3) . . . . ? O1 C14 N13 C13 -170.6(17) . . . . ? O3 C9 N14 C11 -151(7) . . . . ? O3 C9 N14 C10 -27(9) . . . . ? N13 C14 O1 Gd1 -152.4(12) . . . . ? O3 Gd1 O1 C14 -63.3(18) . . . . ? O6 Gd1 O1 C14 89.2(18) . . . . ? O2 Gd1 O1 C14 171.1(19) . . . . ? O5 Gd1 O1 C14 -18(2) . . . . ? O4 Gd1 O1 C14 135.3(17) . . . . ? N3 Gd1 O1 C14 -126.1(17) 1_565 . . . ? N8 Gd1 O1 C14 16.5(18) . . . . ? N11 C21 O2 Gd1 173.4(12) . . . . ? O1 Gd1 O2 C21 162.6(11) . . . . ? O3 Gd1 O2 C21 101.1(11) . . . . ? O6 Gd1 O2 C21 -116.7(11) . . . . ? O5 Gd1 O2 C21 -9.4(13) . . . . ? O4 Gd1 O2 C21 -39.9(11) . . . . ? N3 Gd1 O2 C21 39.7(11) 1_565 . . . ? N8 Gd1 O2 C21 -156.4(10) . . . . ? N14 C9 O3 Gd1 171(4) . . . . ? O1 Gd1 O3 C9 -129(8) . . . . ? O6 Gd1 O3 C9 -175(8) . . . . ? O2 Gd1 O3 C9 -68(8) . . . . ? O5 Gd1 O3 C9 76(8) . . . . ? O4 Gd1 O3 C9 32(8) . . . . ? N3 Gd1 O3 C9 -6(8) 1_565 . . . ? N8 Gd1 O3 C9 152(8) . . . . ? N10 C18 O4 Gd1 178.2(6) . . . . ? O1 Gd1 O4 C18 152.7(7) . . . . ? O3 Gd1 O4 C18 2.6(10) . . . . ? O6 Gd1 O4 C18 -160.2(8) . . . . ? O2 Gd1 O4 C18 117.2(8) . . . . ? O5 Gd1 O4 C18 -43.3(8) . . . . ? N3 Gd1 O4 C18 40.3(8) 1_565 . . . ? N8 Gd1 O4 C18 -103.1(8) . . . . ? N9 C15 O5 Gd1 174.2(7) . . . . ? O1 Gd1 O5 C15 8.7(12) . . . . ? O3 Gd1 O5 C15 52.9(10) . . . . ? O6 Gd1 O5 C15 -88.2(10) . . . . ? O2 Gd1 O5 C15 175.3(9) . . . . ? O4 Gd1 O5 C15 -153.7(10) . . . . ? N3 Gd1 O5 C15 127.6(10) 1_565 . . . ? N8 Gd1 O5 C15 -25.8(9) . . . . ? N12 C26 O6 Gd1 -164.5(9) . . . . ? O1 Gd1 O6 C26 103.4(14) . . . . ? O3 Gd1 O6 C26 148.3(13) . . . . ? O2 Gd1 O6 C26 28.5(13) . . . . ? O5 Gd1 O6 C26 -112.3(13) . . . . ? O4 Gd1 O6 C26 -48.5(13) . . . . ? N3 Gd1 O6 C26 -12.7(15) 1_565 . . . ? N8 Gd1 O6 C26 -177.0(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.163 _refine_diff_density_min -1.560 _refine_diff_density_rms 0.197 _database_code_depnum_ccdc_archive 'CCDC 875832' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl2 #TrackingRef 'shelxl-Ho.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H42 Ho Mo N14 O6' _chemical_formula_weight 907.61 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' Ho Ho -0.2175 4.6783 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.396(3) _cell_length_b 10.996(2) _cell_length_c 21.194(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.86(3) _cell_angle_gamma 90.00 _cell_volume 3820.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1811 _exptl_absorpt_coefficient_mu 2.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6160 _exptl_absorpt_correction_T_max 0.7585 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25824 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6744 _reflns_number_gt 5784 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+10.1778P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6744 _refine_ls_number_parameters 445 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1522 _refine_ls_wR_factor_gt 0.1395 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.194 _refine_ls_shift/su_max 0.058 _refine_ls_shift/su_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_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 C1 C 0.6676(6) 0.2697(8) 0.2176(5) 0.048(2) Uani 1 1 d . . . C2 C 0.6401(6) 0.1897(9) 0.1016(4) 0.058(3) Uani 1 1 d . . . C3 C 0.7587(4) 0.0863(7) 0.1676(4) 0.0354(17) Uani 1 1 d . . . C4 C 0.7972(7) 0.1714(9) 0.0598(4) 0.064(3) Uani 1 1 d . . . C5 C 0.8611(6) 0.3584(9) 0.1082(4) 0.059(2) Uani 1 1 d . . . C6 C 0.7057(6) 0.3861(9) 0.0620(4) 0.054(2) Uani 1 1 d . . . C7 C 0.7413(5) 0.4597(8) 0.1717(4) 0.0400(18) Uani 1 1 d . . . C8 C 0.8329(6) 0.2704(8) 0.2192(5) 0.052(2) Uani 1 1 d . . . C9 C 0.7176(11) 0.4605(14) 0.3846(7) 0.123(6) Uani 1 1 d . . . H9A H 0.7314 0.4591 0.3407 0.185 Uiso 1 1 calc R . . H9B H 0.6731 0.4055 0.3917 0.185 Uiso 1 1 calc R . . H9C H 0.7640 0.4359 0.4096 0.185 Uiso 1 1 calc R . . C10 C 0.6657(12) 0.5910(19) 0.4652(7) 0.161(8) Uani 1 1 d . . . H10A H 0.6773 0.6716 0.4803 0.242 Uiso 1 1 calc R . . H10B H 0.6928 0.5327 0.4920 0.242 Uiso 1 1 calc R . . H10C H 0.6079 0.5770 0.4658 0.242 Uiso 1 1 calc R . . C11 C 0.6966(7) 0.6655(11) 0.3610(6) 0.076(3) Uani 1 1 d . . . H11 H 0.6827 0.7427 0.3753 0.091 Uiso 1 1 calc R . . C12 C 0.9856(14) 0.592(3) 0.3462(8) 0.235(15) Uani 1 1 d . . . H12A H 0.9613 0.6683 0.3566 0.352 Uiso 1 1 calc R . . H12B H 1.0435 0.5962 0.3530 0.352 Uiso 1 1 calc R . . H12C H 0.9633 0.5291 0.3724 0.352 Uiso 1 1 calc R . . C13 C 1.0212(9) 0.4723(18) 0.2586(10) 0.175(10) Uani 1 1 d . . . H13A H 1.0155 0.4709 0.2135 0.262 Uiso 1 1 calc R . . H13B H 1.0059 0.3946 0.2754 0.262 Uiso 1 1 calc R . . H13C H 1.0769 0.4894 0.2701 0.262 Uiso 1 1 calc R . . C14 C 0.9148(8) 0.6155(15) 0.2493(8) 0.109(5) Uani 1 1 d . . . H14 H 0.9082 0.5752 0.2110 0.131 Uiso 1 1 calc R . . C15 C 0.8503(15) 0.966(2) 0.4239(9) 0.236(15) Uani 1 1 d . . . H15A H 0.8697 0.8938 0.4035 0.354 Uiso 1 1 calc R . . H15B H 0.8134 0.9439 0.4568 0.354 Uiso 1 1 calc R . . H15C H 0.8956 1.0099 0.4418 0.354 Uiso 1 1 calc R . . C16 C 0.7827(11) 1.1628(14) 0.3951(7) 0.125(6) Uani 1 1 d . . . H16A H 0.7327 1.1827 0.3734 0.187 Uiso 1 1 calc R . . H16B H 0.8242 1.2201 0.3838 0.187 Uiso 1 1 calc R . . H16C H 0.7745 1.1662 0.4399 0.187 Uiso 1 1 calc R . . C17 C 0.7850(8) 0.9933(11) 0.3264(5) 0.078(3) Uani 1 1 d . . . H17 H 0.7522 1.0406 0.3000 0.094 Uiso 1 1 calc R . . C18 C 0.5869(5) 0.9432(9) 0.2436(4) 0.050(2) Uani 1 1 d . . . H18 H 0.5935 0.9683 0.2021 0.060 Uiso 1 1 calc R . . C19 C 0.4686(6) 1.0724(11) 0.2454(6) 0.083(4) Uani 1 1 d . . . H19A H 0.4821 1.0838 0.2019 0.124 Uiso 1 1 calc R . . H19B H 0.4718 1.1489 0.2671 0.124 Uiso 1 1 calc R . . H19C H 0.4141 1.0409 0.2481 0.124 Uiso 1 1 calc R . . C20 C 0.5121(8) 0.9465(13) 0.3399(5) 0.096(4) Uani 1 1 d . . . H20A H 0.5346 0.8667 0.3459 0.144 Uiso 1 1 calc R . . H20B H 0.4546 0.9444 0.3477 0.144 Uiso 1 1 calc R . . H20C H 0.5381 1.0022 0.3687 0.144 Uiso 1 1 calc R . . C21 C 0.6234(5) 0.7139(7) 0.1000(4) 0.044(2) Uani 1 1 d . . . H21 H 0.6566 0.6506 0.0866 0.053 Uiso 1 1 calc R . . C22 C 0.5003(7) 0.8312(14) 0.0886(7) 0.107(5) Uani 1 1 d . . . H22A H 0.4804 0.8144 0.1301 0.161 Uiso 1 1 calc R . . H22B H 0.4552 0.8363 0.0594 0.161 Uiso 1 1 calc R . . H22C H 0.5294 0.9069 0.0891 0.161 Uiso 1 1 calc R . . C23 C 0.5281(9) 0.6599(13) 0.0161(7) 0.104(5) Uani 1 1 d . . . H23A H 0.5722 0.6086 0.0030 0.156 Uiso 1 1 calc R . . H23B H 0.5118 0.7118 -0.0182 0.156 Uiso 1 1 calc R . . H23C H 0.4828 0.6103 0.0283 0.156 Uiso 1 1 calc R . . C24 C 0.9324(14) 0.8595(19) 0.0060(10) 0.200(8) Uani 1 1 d DU . . H24A H 0.9856 0.8911 0.0162 0.299 Uiso 1 1 calc R . . H24B H 0.8934 0.9246 0.0056 0.299 Uiso 1 1 calc R . . H24C H 0.9334 0.8220 -0.0349 0.299 Uiso 1 1 calc R . . C25 C 0.9728(14) 0.689(2) 0.0562(13) 0.225(9) Uani 1 1 d DU . . H25A H 1.0245 0.7295 0.0571 0.337 Uiso 1 1 calc R . . H25B H 0.9703 0.6344 0.0207 0.337 Uiso 1 1 calc R . . H25C H 0.9666 0.6428 0.0944 0.337 Uiso 1 1 calc R . . C26 C 0.8575(10) 0.7987(17) 0.0915(8) 0.120(4) Uani 1 1 d U . . H26 H 0.8371 0.8756 0.0821 0.144 Uiso 1 1 calc R . . Ho1 Ho 0.75094(2) 0.77561(3) 0.222490(17) 0.03339(15) Uani 1 1 d . . . Mo1 Mo 0.75008(4) 0.27390(6) 0.13854(3) 0.0363(2) Uani 1 1 d . . . N1 N 0.7381(4) 0.5589(6) 0.1880(3) 0.0424(16) Uani 1 1 d . . . N2 N 0.6820(7) 0.4439(9) 0.0213(4) 0.083(3) Uani 1 1 d . . . N3 N 0.5808(6) 0.1442(9) 0.0851(5) 0.088(3) Uani 1 1 d . . . N4 N 0.8234(8) 0.1189(9) 0.0197(4) 0.100(4) Uani 1 1 d . . . N5 N 0.7598(4) -0.0137(6) 0.1826(3) 0.0419(16) Uani 1 1 d . . . N6 N 0.8734(6) 0.2677(9) 0.2631(5) 0.080(3) Uani 1 1 d . . . N7 N 0.6275(6) 0.2657(8) 0.2604(5) 0.074(3) Uani 1 1 d . . . N8 N 0.9203(7) 0.4022(11) 0.0924(5) 0.098(3) Uani 1 1 d . . . N9 N 0.5549(5) 0.7338(8) 0.0694(4) 0.063(2) Uani 1 1 d . . . N10 N 0.5258(4) 0.9866(7) 0.2745(4) 0.0543(19) Uani 1 1 d . . . N11 N 0.6945(6) 0.5784(9) 0.4017(4) 0.078(3) Uani 1 1 d . . . N12 N 0.9693(5) 0.5650(9) 0.2839(5) 0.071(3) Uani 1 1 d . . . N13 N 0.9105(9) 0.7735(13) 0.0509(6) 0.121(3) Uani 1 1 d DU . . N14 N 0.8079(6) 1.0425(8) 0.3778(4) 0.079(3) Uani 1 1 d . . . O1 O 0.8271(5) 0.7668(7) 0.1320(4) 0.079(2) Uani 1 1 d U . . O2 O 0.6462(4) 0.7753(5) 0.1459(3) 0.0507(15) Uani 1 1 d . . . O3 O 0.6371(3) 0.8703(6) 0.2662(3) 0.0521(15) Uani 1 1 d . . . O4 O 0.8008(4) 0.8913(6) 0.3073(3) 0.0573(17) Uani 1 1 d . . . O5 O 0.7145(4) 0.6568(6) 0.3069(3) 0.0629(18) Uani 1 1 d . . . O6 O 0.8734(4) 0.6942(7) 0.2527(5) 0.089(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.058(6) 0.031(5) 0.055(5) -0.008(4) 0.006(4) -0.007(4) C2 0.073(7) 0.045(6) 0.056(6) 0.009(5) -0.025(5) -0.006(5) C3 0.037(4) 0.023(5) 0.046(4) -0.004(3) 0.001(3) 0.002(3) C4 0.110(8) 0.037(5) 0.044(5) 0.001(5) 0.006(5) 0.002(6) C5 0.074(7) 0.045(6) 0.057(6) -0.004(4) 0.022(5) 0.001(5) C6 0.084(7) 0.038(5) 0.038(5) -0.004(4) -0.008(4) 0.008(5) C7 0.048(5) 0.034(5) 0.038(4) 0.000(4) 0.001(3) -0.001(4) C8 0.060(6) 0.034(5) 0.061(6) 0.004(4) -0.010(5) -0.004(4) C9 0.193(17) 0.075(11) 0.100(10) 0.004(9) -0.012(11) -0.004(11) C10 0.21(2) 0.18(2) 0.091(11) 0.032(12) 0.060(12) 0.049(16) C11 0.099(8) 0.052(7) 0.077(8) 0.002(6) 0.010(6) 0.016(6) C12 0.19(2) 0.44(5) 0.073(11) -0.013(19) -0.022(12) -0.02(3) C13 0.066(9) 0.139(18) 0.32(3) -0.092(19) 0.019(12) -0.012(10) C14 0.068(8) 0.109(13) 0.149(13) 0.037(10) -0.028(8) 0.000(8) C15 0.29(3) 0.28(3) 0.134(15) -0.107(18) -0.118(18) 0.17(3) C16 0.197(17) 0.086(11) 0.092(10) -0.026(9) 0.032(10) -0.006(11) C17 0.098(9) 0.060(8) 0.076(7) -0.004(6) 0.003(6) -0.018(7) C18 0.034(4) 0.050(6) 0.065(6) -0.014(5) 0.008(4) 0.005(4) C19 0.052(6) 0.058(7) 0.139(11) -0.001(7) 0.007(6) 0.021(5) C20 0.094(9) 0.115(12) 0.082(8) 0.000(8) 0.047(7) 0.025(8) C21 0.048(5) 0.022(4) 0.063(5) 0.000(4) -0.014(4) -0.001(4) C22 0.072(8) 0.124(12) 0.124(11) -0.028(10) -0.041(8) 0.043(8) C23 0.111(10) 0.076(9) 0.123(11) -0.023(8) -0.057(9) 0.006(8) C24 0.207(11) 0.191(11) 0.201(11) 0.014(9) 0.020(9) -0.002(9) C25 0.223(11) 0.217(12) 0.234(11) 0.004(9) 0.012(9) 0.010(9) C26 0.121(6) 0.128(6) 0.112(6) 0.000(5) 0.027(5) 0.005(5) Ho1 0.0348(2) 0.0202(2) 0.0452(2) -0.00080(15) 0.00037(15) 0.00247(14) Mo1 0.0523(4) 0.0185(4) 0.0381(4) 0.0004(3) -0.0007(3) 0.0004(3) N1 0.049(4) 0.029(4) 0.049(4) -0.003(3) -0.001(3) -0.001(3) N2 0.138(9) 0.058(6) 0.051(5) 0.014(5) -0.016(5) 0.015(6) N3 0.092(7) 0.065(7) 0.106(7) 0.011(6) -0.044(6) -0.020(6) N4 0.182(11) 0.059(7) 0.058(6) -0.016(5) 0.038(6) 0.009(7) N5 0.051(4) 0.016(4) 0.059(4) 0.002(3) 0.005(3) 0.000(3) N6 0.086(7) 0.083(7) 0.071(6) 0.023(5) -0.035(5) -0.018(5) N7 0.086(7) 0.060(6) 0.076(6) -0.006(5) 0.041(5) -0.017(5) N8 0.092(7) 0.097(9) 0.106(8) -0.002(6) 0.037(6) -0.026(7) N9 0.068(5) 0.051(5) 0.071(5) 0.000(4) -0.028(4) 0.000(4) N10 0.041(4) 0.041(5) 0.081(5) -0.002(4) 0.014(4) 0.005(3) N11 0.108(7) 0.065(7) 0.062(5) 0.027(5) 0.014(5) 0.006(5) N12 0.040(4) 0.072(7) 0.101(7) 0.014(5) -0.013(4) 0.017(4) N13 0.124(6) 0.132(6) 0.108(6) 0.013(5) 0.057(5) 0.027(5) N14 0.119(8) 0.055(6) 0.061(5) -0.028(5) -0.022(5) 0.005(5) O1 0.088(4) 0.069(4) 0.082(4) 0.004(3) 0.053(3) 0.002(3) O2 0.051(4) 0.037(4) 0.064(4) -0.005(3) -0.016(3) 0.002(3) O3 0.045(3) 0.049(4) 0.062(4) 0.000(3) 0.011(3) 0.014(3) O4 0.078(4) 0.033(4) 0.060(4) -0.016(3) -0.019(3) 0.006(3) O5 0.099(5) 0.044(4) 0.046(4) 0.007(3) 0.011(3) -0.006(4) O6 0.050(4) 0.055(5) 0.160(8) -0.033(5) -0.033(5) 0.030(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N7 1.129(12) . ? C1 Mo1 2.170(10) . ? C2 N3 1.143(12) . ? C2 Mo1 2.163(10) . ? C3 N5 1.145(10) . ? C3 Mo1 2.157(8) . ? C4 N4 1.119(12) . ? C4 Mo1 2.166(10) . ? C5 N8 1.138(12) . ? C5 Mo1 2.151(10) . ? C6 N2 1.136(11) . ? C6 Mo1 2.156(9) . ? C7 N1 1.145(10) . ? C7 Mo1 2.166(9) . ? C8 N6 1.136(12) . ? C8 Mo1 2.167(10) . ? C9 N11 1.401(17) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 N11 1.441(16) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O5 1.193(12) . ? C11 N11 1.289(14) . ? C11 H11 0.9300 . ? C12 N12 1.374(17) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N12 1.437(18) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 O6 1.103(16) . ? C14 N12 1.274(14) . ? C14 H14 0.9300 . ? C15 N14 1.46(2) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N14 1.435(16) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O4 1.221(13) . ? C17 N14 1.268(13) . ? C17 H17 0.9300 . ? C18 O3 1.240(10) . ? C18 N10 1.296(10) . ? C18 H18 0.9300 . ? C19 N10 1.461(13) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N10 1.474(13) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 O2 1.237(10) . ? C21 N9 1.308(11) . ? C21 H21 0.9300 . ? C22 N9 1.457(14) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 N9 1.455(13) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N13 1.393(10) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N13 1.387(10) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O1 1.059(17) . ? C26 N13 1.263(18) . ? C26 H26 0.9300 . ? Ho1 O6 2.281(7) . ? Ho1 O5 2.300(6) . ? Ho1 O1 2.305(7) . ? Ho1 O4 2.339(6) . ? Ho1 O3 2.341(6) . ? Ho1 O2 2.346(6) . ? Ho1 N5 2.471(6) 1_565 ? Ho1 N1 2.501(7) . ? N5 Ho1 2.471(6) 1_545 ? 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 N7 C1 Mo1 176.9(10) . . ? N3 C2 Mo1 176.6(10) . . ? N5 C3 Mo1 177.1(7) . . ? N4 C4 Mo1 178.4(12) . . ? N8 C5 Mo1 179.3(11) . . ? N2 C6 Mo1 179.2(9) . . ? N1 C7 Mo1 178.1(7) . . ? N6 C8 Mo1 177.0(10) . . ? N11 C9 H9A 109.5 . . ? N11 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N11 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N11 C10 H10A 109.5 . . ? N11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 N11 126.4(12) . . ? O5 C11 H11 116.8 . . ? N11 C11 H11 116.8 . . ? N12 C12 H12A 109.5 . . ? N12 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N12 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N12 C13 H13A 109.5 . . ? N12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O6 C14 N12 137.0(18) . . ? O6 C14 H14 111.5 . . ? N12 C14 H14 111.5 . . ? N14 C15 H15A 109.5 . . ? N14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N14 C16 H16A 109.5 . . ? N14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O4 C17 N14 128.0(12) . . ? O4 C17 H17 116.0 . . ? N14 C17 H17 116.0 . . ? O3 C18 N10 123.8(9) . . ? O3 C18 H18 118.1 . . ? N10 C18 H18 118.1 . . ? N10 C19 H19A 109.5 . . ? N10 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N10 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N10 C20 H20A 109.5 . . ? N10 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N10 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O2 C21 N9 123.0(8) . . ? O2 C21 H21 118.5 . . ? N9 C21 H21 118.5 . . ? N9 C22 H22A 109.5 . . ? N9 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N9 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N9 C23 H23A 109.5 . . ? N9 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N9 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N13 C24 H24A 109.5 . . ? N13 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N13 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N13 C25 H25A 109.5 . . ? N13 C25 H25B 109.4 . . ? H25A C25 H25B 109.5 . . ? N13 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O1 C26 N13 145(2) . . ? O1 C26 H26 107.6 . . ? N13 C26 H26 107.6 . . ? O6 Ho1 O5 78.2(3) . . ? O6 Ho1 O1 74.4(3) . . ? O5 Ho1 O1 140.6(3) . . ? O6 Ho1 O4 72.7(3) . . ? O5 Ho1 O4 78.7(2) . . ? O1 Ho1 O4 118.3(3) . . ? O6 Ho1 O3 140.1(3) . . ? O5 Ho1 O3 74.2(2) . . ? O1 Ho1 O3 142.5(3) . . ? O4 Ho1 O3 74.1(2) . . ? O6 Ho1 O2 145.7(3) . . ? O5 Ho1 O2 110.0(2) . . ? O1 Ho1 O2 79.9(3) . . ? O4 Ho1 O2 140.9(2) . . ? O3 Ho1 O2 72.2(2) . . ? O6 Ho1 N5 114.1(3) . 1_565 ? O5 Ho1 N5 144.6(2) . 1_565 ? O1 Ho1 N5 73.7(2) . 1_565 ? O4 Ho1 N5 74.4(2) . 1_565 ? O3 Ho1 N5 76.7(2) . 1_565 ? O2 Ho1 N5 79.1(2) . 1_565 ? O6 Ho1 N1 77.2(2) . . ? O5 Ho1 N1 70.4(2) . . ? O1 Ho1 N1 76.2(3) . . ? O4 Ho1 N1 140.4(2) . . ? O3 Ho1 N1 118.4(2) . . ? O2 Ho1 N1 74.8(2) . . ? N5 Ho1 N1 143.0(2) 1_565 . ? C5 Mo1 C6 78.8(4) . . ? C5 Mo1 C3 116.5(3) . . ? C6 Mo1 C3 141.4(3) . . ? C5 Mo1 C2 141.4(4) . . ? C6 Mo1 C2 72.7(4) . . ? C3 Mo1 C2 75.2(3) . . ? C5 Mo1 C4 71.4(4) . . ? C6 Mo1 C4 80.7(4) . . ? C3 Mo1 C4 72.5(3) . . ? C2 Mo1 C4 78.7(4) . . ? C5 Mo1 C7 75.6(3) . . ? C6 Mo1 C7 71.4(3) . . ? C3 Mo1 C7 144.5(3) . . ? C2 Mo1 C7 117.5(3) . . ? C4 Mo1 C7 140.1(3) . . ? C5 Mo1 C8 73.8(4) . . ? C6 Mo1 C8 143.5(3) . . ? C3 Mo1 C8 73.8(3) . . ? C2 Mo1 C8 141.9(3) . . ? C4 Mo1 C8 111.8(4) . . ? C7 Mo1 C8 78.7(3) . . ? C5 Mo1 C1 141.3(3) . . ? C6 Mo1 C1 112.7(4) . . ? C3 Mo1 C1 78.3(3) . . ? C2 Mo1 C1 75.2(4) . . ? C4 Mo1 C1 144.9(4) . . ? C7 Mo1 C1 74.0(3) . . ? C8 Mo1 C1 77.3(4) . . ? C7 N1 Ho1 172.5(6) . . ? C3 N5 Ho1 174.2(6) . 1_545 ? C21 N9 C23 122.6(9) . . ? C21 N9 C22 120.8(8) . . ? C23 N9 C22 116.7(9) . . ? C18 N10 C19 121.4(9) . . ? C18 N10 C20 119.7(8) . . ? C19 N10 C20 118.9(8) . . ? C11 N11 C9 120.3(11) . . ? C11 N11 C10 124.5(13) . . ? C9 N11 C10 115.1(12) . . ? C14 N12 C12 125.7(17) . . ? C14 N12 C13 120.6(14) . . ? C12 N12 C13 113.7(15) . . ? C26 N13 C25 127.3(18) . . ? C26 N13 C24 120.3(18) . . ? C25 N13 C24 108.4(18) . . ? C17 N14 C16 122.1(12) . . ? C17 N14 C15 117.5(12) . . ? C16 N14 C15 119.7(11) . . ? C26 O1 Ho1 158.1(12) . . ? C21 O2 Ho1 138.9(6) . . ? C18 O3 Ho1 131.5(6) . . ? C17 O4 Ho1 132.9(7) . . ? C11 O5 Ho1 140.6(8) . . ? C14 O6 Ho1 146.1(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 C5 Mo1 C6 -161(100) . . . . ? N8 C5 Mo1 C3 -18(97) . . . . ? N8 C5 Mo1 C2 -118(97) . . . . ? N8 C5 Mo1 C4 -77(97) . . . . ? N8 C5 Mo1 C7 126(97) . . . . ? N8 C5 Mo1 C8 44(97) . . . . ? N8 C5 Mo1 C1 87(97) . . . . ? N2 C6 Mo1 C5 115(74) . . . . ? N2 C6 Mo1 C3 -4(75) . . . . ? N2 C6 Mo1 C2 -39(74) . . . . ? N2 C6 Mo1 C4 42(74) . . . . ? N2 C6 Mo1 C7 -167(100) . . . . ? N2 C6 Mo1 C8 157(74) . . . . ? N2 C6 Mo1 C1 -104(74) . . . . ? N5 C3 Mo1 C5 -161(14) . . . . ? N5 C3 Mo1 C6 -55(14) . . . . ? N5 C3 Mo1 C2 -21(14) . . . . ? N5 C3 Mo1 C4 -104(14) . . . . ? N5 C3 Mo1 C7 96(14) . . . . ? N5 C3 Mo1 C8 137(14) . . . . ? N5 C3 Mo1 C1 57(14) . . . . ? N3 C2 Mo1 C5 180(100) . . . . ? N3 C2 Mo1 C6 -136(16) . . . . ? N3 C2 Mo1 C3 66(16) . . . . ? N3 C2 Mo1 C4 140(16) . . . . ? N3 C2 Mo1 C7 -79(16) . . . . ? N3 C2 Mo1 C8 29(16) . . . . ? N3 C2 Mo1 C1 -16(16) . . . . ? N4 C4 Mo1 C5 36(34) . . . . ? N4 C4 Mo1 C6 117(35) . . . . ? N4 C4 Mo1 C3 -91(35) . . . . ? N4 C4 Mo1 C2 -169(35) . . . . ? N4 C4 Mo1 C7 71(35) . . . . ? N4 C4 Mo1 C8 -28(35) . . . . ? N4 C4 Mo1 C1 -127(34) . . . . ? N1 C7 Mo1 C5 24(23) . . . . ? N1 C7 Mo1 C6 -58(23) . . . . ? N1 C7 Mo1 C3 140(23) . . . . ? N1 C7 Mo1 C2 -116(23) . . . . ? N1 C7 Mo1 C4 -10(23) . . . . ? N1 C7 Mo1 C8 100(23) . . . . ? N1 C7 Mo1 C1 -180(100) . . . . ? N6 C8 Mo1 C5 161(17) . . . . ? N6 C8 Mo1 C6 119(16) . . . . ? N6 C8 Mo1 C3 -74(17) . . . . ? N6 C8 Mo1 C2 -37(17) . . . . ? N6 C8 Mo1 C4 -137(17) . . . . ? N6 C8 Mo1 C7 83(17) . . . . ? N6 C8 Mo1 C1 8(17) . . . . ? N7 C1 Mo1 C5 -61(15) . . . . ? N7 C1 Mo1 C6 -161(15) . . . . ? N7 C1 Mo1 C3 58(15) . . . . ? N7 C1 Mo1 C2 135(15) . . . . ? N7 C1 Mo1 C4 92(15) . . . . ? N7 C1 Mo1 C7 -100(15) . . . . ? N7 C1 Mo1 C8 -18(15) . . . . ? Mo1 C7 N1 Ho1 -47(26) . . . . ? O6 Ho1 N1 C7 -27(5) . . . . ? O5 Ho1 N1 C7 -108(5) . . . . ? O1 Ho1 N1 C7 50(5) . . . . ? O4 Ho1 N1 C7 -68(5) . . . . ? O3 Ho1 N1 C7 -167(5) . . . . ? O2 Ho1 N1 C7 133(5) . . . . ? N5 Ho1 N1 C7 87(5) 1_565 . . . ? Mo1 C3 N5 Ho1 -50(18) . . . 1_545 ? O2 C21 N9 C23 -179.1(11) . . . . ? O2 C21 N9 C22 -0.4(16) . . . . ? O3 C18 N10 C19 180.0(9) . . . . ? O3 C18 N10 C20 -1.6(15) . . . . ? O5 C11 N11 C9 3(2) . . . . ? O5 C11 N11 C10 -174.5(15) . . . . ? O6 C14 N12 C12 10(3) . . . . ? O6 C14 N12 C13 -169.7(19) . . . . ? O1 C26 N13 C25 -21(5) . . . . ? O1 C26 N13 C24 -176(3) . . . . ? O4 C17 N14 C16 -178.3(13) . . . . ? O4 C17 N14 C15 -8(2) . . . . ? N13 C26 O1 Ho1 162(2) . . . . ? O6 Ho1 O1 C26 -121(3) . . . . ? O5 Ho1 O1 C26 -168(3) . . . . ? O4 Ho1 O1 C26 -61(3) . . . . ? O3 Ho1 O1 C26 40(3) . . . . ? O2 Ho1 O1 C26 82(3) . . . . ? N5 Ho1 O1 C26 1(3) 1_565 . . . ? N1 Ho1 O1 C26 159(3) . . . . ? N9 C21 O2 Ho1 173.3(7) . . . . ? O6 Ho1 O2 C21 11.7(12) . . . . ? O5 Ho1 O2 C21 -86.8(9) . . . . ? O1 Ho1 O2 C21 53.6(9) . . . . ? O4 Ho1 O2 C21 176.6(8) . . . . ? O3 Ho1 O2 C21 -151.8(10) . . . . ? N5 Ho1 O2 C21 128.8(9) 1_565 . . . ? N1 Ho1 O2 C21 -24.7(9) . . . . ? N10 C18 O3 Ho1 179.1(6) . . . . ? O6 Ho1 O3 C18 153.5(7) . . . . ? O5 Ho1 O3 C18 -158.6(8) . . . . ? O1 Ho1 O3 C18 3.0(10) . . . . ? O4 Ho1 O3 C18 119.0(8) . . . . ? O2 Ho1 O3 C18 -40.9(8) . . . . ? N5 Ho1 O3 C18 41.7(8) 1_565 . . . ? N1 Ho1 O3 C18 -101.9(8) . . . . ? N14 C17 O4 Ho1 169.9(9) . . . . ? O6 Ho1 O4 C17 160.8(11) . . . . ? O5 Ho1 O4 C17 -118.1(10) . . . . ? O1 Ho1 O4 C17 100.0(10) . . . . ? O3 Ho1 O4 C17 -41.5(10) . . . . ? O2 Ho1 O4 C17 -10.3(12) . . . . ? N5 Ho1 O4 C17 38.7(10) 1_565 . . . ? N1 Ho1 O4 C17 -157.0(9) . . . . ? N11 C11 O5 Ho1 -164.8(9) . . . . ? O6 Ho1 O5 C11 103.8(12) . . . . ? O1 Ho1 O5 C11 150.6(12) . . . . ? O4 Ho1 O5 C11 29.4(12) . . . . ? O3 Ho1 O5 C11 -47.1(12) . . . . ? O2 Ho1 O5 C11 -110.9(12) . . . . ? N5 Ho1 O5 C11 -11.5(14) 1_565 . . . ? N1 Ho1 O5 C11 -175.8(13) . . . . ? N12 C14 O6 Ho1 -150.8(14) . . . . ? O5 Ho1 O6 C14 84(2) . . . . ? O1 Ho1 O6 C14 -67(2) . . . . ? O4 Ho1 O6 C14 166(2) . . . . ? O3 Ho1 O6 C14 131(2) . . . . ? O2 Ho1 O6 C14 -24(2) . . . . ? N5 Ho1 O6 C14 -131(2) 1_565 . . . ? N1 Ho1 O6 C14 12(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.363 _refine_diff_density_min -1.288 _refine_diff_density_rms 0.216 _database_code_depnum_ccdc_archive 'CCDC 881383' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelx #TrackingRef '12022701.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H42 Er Mo N14 O6' _chemical_formula_weight 909.94 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' Er Er -0.2586 4.9576 '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' 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.369(5) _cell_length_b 10.983(3) _cell_length_c 21.234(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.124(14) _cell_angle_gamma 90.00 _cell_volume 3816.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 566(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1815 _exptl_absorpt_coefficient_mu 2.567 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6020 _exptl_absorpt_correction_T_max 0.7481 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 566(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28462 _diffrn_reflns_av_R_equivalents 0.1213 _diffrn_reflns_av_sigmaI/netI 0.0921 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6510 _reflns_number_gt 4866 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1270P)^2^+42.5795P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6510 _refine_ls_number_parameters 445 _refine_ls_number_restraints 211 _refine_ls_R_factor_all 0.1173 _refine_ls_R_factor_gt 0.0933 _refine_ls_wR_factor_ref 0.2534 _refine_ls_wR_factor_gt 0.2325 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.003 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 C1 C 0.2430(9) 0.9138(13) 0.3319(6) 0.046(3) Uani 1 1 d . . . C2 C 0.2054(18) 0.829(3) 0.4382(13) 0.114(7) Uani 1 1 d U . . C3 C 0.1399(15) 0.6406(17) 0.3918(10) 0.084(6) Uani 1 1 d . . . C4 C 0.2961(14) 0.6146(17) 0.4386(8) 0.075(5) Uani 1 1 d . . . C5 C 0.3604(12) 0.810(2) 0.3990(12) 0.091(7) Uani 1 1 d . . . C6 C 0.3327(10) 0.7293(14) 0.2813(8) 0.055(4) Uani 1 1 d . . . C7 C 0.1666(11) 0.7305(14) 0.2808(9) 0.061(4) Uani 1 1 d . . . C8 C 0.2567(9) 0.5397(12) 0.3284(6) 0.042(3) Uani 1 1 d . . . C9 C 0.3742(11) 0.2857(15) 0.4001(10) 0.069(5) Uani 1 1 d . . . H9 H 0.3422 0.3506 0.4130 0.082 Uiso 1 1 calc R . . C10 C 0.5015(15) 0.172(3) 0.4087(14) 0.137(12) Uani 1 1 d . . . H10A H 0.4793 0.0916 0.4145 0.206 Uiso 1 1 calc R . . H10B H 0.5523 0.1784 0.4318 0.206 Uiso 1 1 calc R . . H10C H 0.5106 0.1852 0.3648 0.206 Uiso 1 1 calc R . . C11 C 0.472(2) 0.341(3) 0.4804(13) 0.139(12) Uani 1 1 d . . . H11A H 0.5147 0.3926 0.4646 0.209 Uiso 1 1 calc R . . H11B H 0.4935 0.2938 0.5149 0.209 Uiso 1 1 calc R . . H11C H 0.4280 0.3909 0.4946 0.209 Uiso 1 1 calc R . . C12 C 0.4142(12) 0.0554(16) 0.2555(9) 0.071(5) Uani 1 1 d . . . H12 H 0.4088 0.0305 0.2971 0.085 Uiso 1 1 calc R . . C13 C 0.4863(15) 0.053(3) 0.1571(12) 0.137(11) Uani 1 1 d . . . H13A H 0.4402 0.0286 0.1314 0.205 Uiso 1 1 calc R . . H13B H 0.5347 0.0141 0.1421 0.205 Uiso 1 1 calc R . . H13C H 0.4926 0.1395 0.1552 0.205 Uiso 1 1 calc R . . C14 C 0.5320(13) -0.0695(19) 0.2638(14) 0.114(9) Uani 1 1 d . . . H14A H 0.5023 -0.1136 0.2950 0.170 Uiso 1 1 calc R . . H14B H 0.5733 -0.0205 0.2842 0.170 Uiso 1 1 calc R . . H14C H 0.5573 -0.1258 0.2357 0.170 Uiso 1 1 calc R . . C15 C 0.155(3) 0.042(4) 0.0761(17) 0.22(2) Uani 1 1 d . . . H15A H 0.0973 0.0304 0.0782 0.337 Uiso 1 1 calc R . . H15B H 0.1728 0.0258 0.0340 0.337 Uiso 1 1 calc R . . H15C H 0.1688 0.1241 0.0873 0.337 Uiso 1 1 calc R . . C16 C 0.224(3) -0.165(3) 0.1049(14) 0.176(17) Uani 1 1 d . . . H16A H 0.2804 -0.1628 0.0926 0.264 Uiso 1 1 calc R . . H16B H 0.1912 -0.1971 0.0709 0.264 Uiso 1 1 calc R . . H16C H 0.2192 -0.2167 0.1412 0.264 Uiso 1 1 calc R . . C17 C 0.2173(19) 0.0104(19) 0.1743(10) 0.111(9) Uani 1 1 d U . . H17 H 0.2503 -0.0350 0.2017 0.134 Uiso 1 1 calc R . . C18 C 0.331(2) 0.405(4) 0.0372(14) 0.181(16) Uani 1 1 d U . . H18A H 0.3821 0.3613 0.0367 0.272 Uiso 1 1 calc R . . H18B H 0.3379 0.4823 0.0167 0.272 Uiso 1 1 calc R . . H18C H 0.2899 0.3587 0.0154 0.272 Uiso 1 1 calc R . . C19 C 0.278(2) 0.543(2) 0.1182(12) 0.128(10) Uani 1 1 d U . . H19A H 0.2191 0.5438 0.1146 0.192 Uiso 1 1 calc R . . H19B H 0.2996 0.6037 0.0906 0.192 Uiso 1 1 calc R . . H19C H 0.2941 0.5609 0.1609 0.192 Uiso 1 1 calc R . . C20 C 0.3075(14) 0.336(2) 0.1413(12) 0.094(7) Uani 1 1 d U . . H20 H 0.3276 0.2612 0.1286 0.113 Uiso 1 1 calc R . . C21 C 0.017(3) 0.418(5) 0.1541(16) 0.23(2) Uani 1 1 d U . . H21A H 0.0434 0.4820 0.1315 0.338 Uiso 1 1 calc R . . H21B H -0.0404 0.4180 0.1437 0.338 Uiso 1 1 calc R . . H21C H 0.0402 0.3410 0.1426 0.338 Uiso 1 1 calc R . . C22 C -0.0256(19) 0.528(3) 0.2524(19) 0.171(15) Uani 1 1 d U . . H22A H -0.0169 0.5244 0.2972 0.256 Uiso 1 1 calc R . . H22B H -0.0817 0.5103 0.2423 0.256 Uiso 1 1 calc R . . H22C H -0.0126 0.6086 0.2378 0.256 Uiso 1 1 calc R . . C23 C 0.0854(19) 0.386(3) 0.2509(19) 0.151(12) Uani 1 1 d U . . H23 H 0.0957 0.4260 0.2887 0.181 Uiso 1 1 calc R . . C24 C 0.1330(17) 0.279(3) 0.4001(13) 0.109(4) Uani 1 1 d U . . H24 H 0.1479 0.3594 0.4067 0.131 Uiso 1 1 calc R . . C25 C 0.074(2) 0.130(3) 0.4814(16) 0.182(10) Uani 1 1 d DU . . H25A H 0.0994 0.0615 0.4612 0.273 Uiso 1 1 calc R . . H25B H 0.0190 0.1091 0.4917 0.273 Uiso 1 1 calc R . . H25C H 0.1043 0.1496 0.5193 0.273 Uiso 1 1 calc R . . C26 C 0.007(2) 0.327(4) 0.4740(17) 0.165(9) Uani 1 1 d U . . H26A H -0.0293 0.2776 0.4987 0.248 Uiso 1 1 calc R . . H26B H -0.0248 0.3711 0.4431 0.248 Uiso 1 1 calc R . . H26C H 0.0355 0.3827 0.5011 0.248 Uiso 1 1 calc R . . Er1 Er 0.24937(4) 0.22484(5) 0.27789(3) 0.0374(2) Uani 1 1 d . . . Mo1 Mo 0.25007(8) 0.72655(9) 0.36150(5) 0.0393(3) Uani 1 1 d . . . N1 N 0.4438(11) 0.2627(17) 0.4319(9) 0.094(6) Uani 1 1 d . . . N2 N 0.4722(9) 0.0141(15) 0.2260(8) 0.074(4) Uani 1 1 d . . . N3 N 0.3080(14) 0.424(2) 0.1007(9) 0.111(6) Uani 1 1 d U . . N4 N 0.0285(10) 0.4371(18) 0.2210(11) 0.099(6) Uani 1 1 d U . . N5 N 0.2582(8) 0.4409(9) 0.3118(5) 0.050(3) Uani 1 1 d . . . N6 N 0.3720(11) 0.7382(14) 0.2389(8) 0.074(4) Uani 1 1 d . . . N7 N 0.3194(13) 0.561(2) 0.4779(8) 0.107(6) Uani 1 1 d . . . N8 N 0.4194(12) 0.8598(17) 0.4148(9) 0.098(6) Uani 1 1 d . . . N9 N 0.1752(14) 0.884(2) 0.4817(9) 0.112(6) Uani 1 1 d U . . N10 N 0.2430(8) 1.0142(9) 0.3179(5) 0.048(3) Uani 1 1 d . . . N11 N 0.0783(14) 0.600(2) 0.4057(11) 0.126(8) Uani 1 1 d . . . N12 N 0.1248(11) 0.7323(15) 0.2389(8) 0.081(5) Uani 1 1 d . . . N13 N 0.1970(13) -0.043(2) 0.1202(8) 0.103(6) Uani 1 1 d U . . N14 N 0.0738(16) 0.237(2) 0.4379(11) 0.126(5) Uani 1 1 d DU . . O1 O 0.3613(7) 0.1294(13) 0.2333(6) 0.079(4) Uani 1 1 d . . . O2 O 0.3506(8) 0.2263(10) 0.3551(7) 0.077(4) Uani 1 1 d . . . O3 O 0.1667(9) 0.2306(12) 0.3621(7) 0.082(3) Uani 1 1 d U . . O4 O 0.1276(10) 0.3066(13) 0.2464(10) 0.113(6) Uani 1 1 d U . . O5 O 0.2836(11) 0.3441(13) 0.1927(7) 0.096(5) Uani 1 1 d U . . O6 O 0.1984(8) 0.1096(12) 0.1924(7) 0.083(4) Uani 1 1 d U . . 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 C1 0.051(9) 0.039(8) 0.046(7) -0.005(6) 0.001(6) 0.011(6) C2 0.125(10) 0.107(10) 0.111(10) 0.005(8) 0.010(8) 0.003(8) C3 0.095(16) 0.048(11) 0.110(15) 0.005(10) 0.041(12) -0.003(10) C4 0.110(16) 0.052(10) 0.062(11) 0.018(8) -0.008(10) 0.001(10) C5 0.050(11) 0.082(15) 0.14(2) 0.008(13) -0.019(12) 0.009(11) C6 0.060(10) 0.037(8) 0.070(10) 0.001(7) 0.011(8) -0.003(7) C7 0.062(10) 0.040(8) 0.081(12) 0.007(8) -0.010(9) -0.014(8) C8 0.057(9) 0.035(8) 0.034(6) 0.006(5) -0.008(6) 0.010(6) C9 0.066(11) 0.037(9) 0.102(14) 0.001(8) -0.016(10) -0.005(8) C10 0.070(15) 0.17(3) 0.17(3) -0.06(2) -0.041(15) 0.056(17) C11 0.16(3) 0.13(2) 0.12(2) -0.004(18) -0.070(19) -0.04(2) C12 0.074(13) 0.048(10) 0.092(13) 0.009(8) 0.024(10) 0.018(9) C13 0.083(17) 0.21(3) 0.12(2) -0.02(2) 0.057(15) 0.02(2) C14 0.055(12) 0.049(12) 0.24(3) 0.009(15) -0.025(15) -0.009(10) C15 0.26(5) 0.25(5) 0.17(3) 0.06(4) 0.05(3) 0.13(4) C16 0.33(5) 0.078(19) 0.12(2) 0.017(17) 0.05(3) -0.04(3) C17 0.20(3) 0.044(11) 0.088(14) -0.015(10) -0.033(15) 0.000(14) C18 0.20(3) 0.22(4) 0.12(2) 0.04(2) 0.08(2) 0.00(3) C19 0.22(3) 0.052(13) 0.116(19) -0.008(12) 0.032(19) 0.006(17) C20 0.088(15) 0.103(17) 0.093(16) 0.006(13) 0.023(12) 0.028(13) C21 0.20(4) 0.37(6) 0.11(2) -0.02(3) -0.01(2) -0.10(4) C22 0.11(2) 0.09(2) 0.31(4) -0.07(3) 0.00(3) 0.017(18) C23 0.11(2) 0.09(2) 0.25(3) 0.06(2) -0.03(2) -0.004(18) C24 0.117(7) 0.105(7) 0.107(7) -0.002(6) 0.026(6) 0.000(6) C25 0.184(12) 0.179(13) 0.183(12) 0.002(9) 0.006(9) -0.001(9) C26 0.167(12) 0.163(12) 0.167(12) 0.006(9) 0.010(9) -0.007(9) Er1 0.0473(4) 0.0180(3) 0.0468(4) -0.0011(2) -0.0001(2) 0.0016(2) Mo1 0.0627(8) 0.0166(5) 0.0387(6) 0.0002(4) -0.0015(5) 0.0004(5) N1 0.084(12) 0.099(13) 0.098(13) -0.018(10) -0.045(10) 0.034(10) N2 0.045(8) 0.075(10) 0.102(11) 0.001(8) 0.015(7) 0.014(8) N3 0.129(17) 0.118(17) 0.087(13) 0.004(12) -0.013(12) 0.012(14) N4 0.048(9) 0.087(13) 0.158(17) 0.025(12) -0.048(10) -0.008(9) N5 0.084(9) 0.016(6) 0.050(7) -0.002(5) -0.009(6) 0.003(6) N6 0.092(12) 0.057(9) 0.073(10) 0.006(7) 0.021(9) 0.002(8) N7 0.134(17) 0.110(16) 0.075(11) 0.016(11) -0.019(11) 0.022(13) N8 0.084(13) 0.077(12) 0.132(15) 0.000(10) -0.035(11) -0.031(10) N9 0.124(9) 0.114(9) 0.099(8) -0.011(7) 0.016(7) 0.004(8) N10 0.077(9) 0.016(6) 0.052(7) 0.006(5) 0.005(6) 0.015(5) N11 0.101(17) 0.13(2) 0.150(19) 0.008(15) 0.040(14) -0.003(15) N12 0.089(12) 0.081(11) 0.071(10) -0.001(8) -0.034(9) -0.003(9) N13 0.130(17) 0.106(15) 0.072(11) -0.017(10) 0.003(10) 0.011(13) N14 0.132(8) 0.125(8) 0.122(7) -0.001(6) 0.029(6) -0.007(6) O1 0.055(7) 0.085(9) 0.098(9) -0.009(7) 0.014(6) 0.012(7) O2 0.072(8) 0.043(6) 0.115(10) -0.016(6) -0.046(7) 0.011(6) O3 0.092(6) 0.066(6) 0.089(6) -0.006(5) 0.040(5) 0.009(5) O4 0.076(10) 0.050(8) 0.211(18) -0.031(10) -0.024(10) 0.021(8) O5 0.155(14) 0.061(9) 0.072(8) 0.012(7) 0.006(9) 0.007(9) O6 0.080(9) 0.056(8) 0.113(10) -0.010(7) -0.027(7) -0.002(7) _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 C1 N10 1.143(17) . ? C1 Mo1 2.153(15) . ? C2 N9 1.22(3) . ? C2 Mo1 2.12(3) . ? C3 N11 1.14(3) . ? C3 Mo1 2.15(2) . ? C4 N7 1.08(2) . ? C4 Mo1 2.171(17) . ? C5 N8 1.15(2) . ? C5 Mo1 2.16(2) . ? C6 N6 1.12(2) . ? C6 Mo1 2.195(17) . ? C7 N12 1.11(2) . ? C7 Mo1 2.172(18) . ? C8 N5 1.142(17) . ? C8 Mo1 2.172(14) . ? C9 O2 1.21(2) . ? C9 N1 1.34(2) . ? C9 H9 0.9300 . ? C10 N1 1.47(3) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N1 1.42(3) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N2 1.23(2) . ? C12 O1 1.27(2) . ? C12 H12 0.9300 . ? C13 N2 1.54(3) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N2 1.55(3) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N13 1.48(4) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N13 1.46(4) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O6 1.20(2) . ? C17 N13 1.33(3) . ? C17 H17 0.9300 . ? C18 N3 1.42(3) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N3 1.45(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 O5 1.17(2) . ? C20 N3 1.30(3) . ? C20 H20 0.9300 . ? C21 N4 1.45(3) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N4 1.50(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 O4 1.12(3) . ? C23 N4 1.25(3) . ? C23 H23 0.9300 . ? C24 O3 1.12(3) . ? C24 N14 1.35(3) . ? C24 H24 0.9300 . ? C25 N14 1.496(10) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 N14 1.67(4) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? Er1 O3 2.265(12) . ? Er1 O4 2.275(15) . ? Er1 O2 2.309(11) . ? Er1 O5 2.312(14) . ? Er1 O1 2.328(12) . ? Er1 O6 2.353(13) . ? Er1 N10 2.467(10) 1_545 ? Er1 N5 2.483(10) . ? N10 Er1 2.467(10) 1_565 ? 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 N10 C1 Mo1 176.4(13) . . ? N9 C2 Mo1 176(3) . . ? N11 C3 Mo1 176(2) . . ? N7 C4 Mo1 178(2) . . ? N8 C5 Mo1 175(2) . . ? N6 C6 Mo1 174.9(15) . . ? N12 C7 Mo1 179.0(19) . . ? N5 C8 Mo1 178.2(14) . . ? O2 C9 N1 123.5(18) . . ? O2 C9 H9 118.3 . . ? N1 C9 H9 118.3 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 O1 124.9(18) . . ? N2 C12 H12 117.6 . . ? O1 C12 H12 117.6 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N13 C15 H15A 109.5 . . ? N13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N13 C16 H16A 109.5 . . ? N13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O6 C17 N13 128(2) . . ? O6 C17 H17 116.0 . . ? N13 C17 H17 116.0 . . ? N3 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O5 C20 N3 125(2) . . ? O5 C20 H20 117.5 . . ? N3 C20 H20 117.5 . . ? N4 C21 H21A 109.5 . . ? N4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 H22A 109.5 . . ? N4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O4 C23 N4 140(4) . . ? O4 C23 H23 110.1 . . ? N4 C23 H23 110.1 . . ? O3 C24 N14 130(3) . . ? O3 C24 H24 115.2 . . ? N14 C24 H24 115.2 . . ? N14 C25 H25A 109.5 . . ? N14 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N14 C25 H25C 109.4 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N14 C26 H26A 109.5 . . ? N14 C26 H26B 109.4 . . ? H26A C26 H26B 109.5 . . ? N14 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O3 Er1 O4 71.8(7) . . ? O3 Er1 O2 82.5(6) . . ? O4 Er1 O2 145.0(5) . . ? O3 Er1 O5 139.5(5) . . ? O4 Er1 O5 76.7(7) . . ? O2 Er1 O5 111.8(6) . . ? O3 Er1 O1 145.2(5) . . ? O4 Er1 O1 138.6(6) . . ? O2 Er1 O1 74.5(5) . . ? O5 Er1 O1 74.4(5) . . ? O3 Er1 O6 114.6(5) . . ? O4 Er1 O6 71.9(5) . . ? O2 Er1 O6 142.3(4) . . ? O5 Er1 O6 77.8(5) . . ? O1 Er1 O6 73.4(5) . . ? O3 Er1 N10 74.0(4) . 1_545 ? O4 Er1 N10 115.4(5) . 1_545 ? O2 Er1 N10 78.2(4) . 1_545 ? O5 Er1 N10 144.4(4) . 1_545 ? O1 Er1 N10 75.9(4) . 1_545 ? O6 Er1 N10 75.2(4) . 1_545 ? O3 Er1 N5 77.1(5) . . ? O4 Er1 N5 75.7(5) . . ? O2 Er1 N5 75.6(4) . . ? O5 Er1 N5 70.8(5) . . ? O1 Er1 N5 120.4(5) . . ? O6 Er1 N5 139.1(4) . . ? N10 Er1 N5 143.0(4) 1_545 . ? C2 Mo1 C3 72.5(10) . . ? C2 Mo1 C1 72.5(8) . . ? C3 Mo1 C1 117.8(7) . . ? C2 Mo1 C5 77.9(10) . . ? C3 Mo1 C5 141.0(9) . . ? C1 Mo1 C5 75.1(7) . . ? C2 Mo1 C4 80.9(9) . . ? C3 Mo1 C4 78.8(9) . . ? C1 Mo1 C4 141.0(6) . . ? C5 Mo1 C4 71.8(8) . . ? C2 Mo1 C8 140.4(8) . . ? C3 Mo1 C8 74.3(6) . . ? C1 Mo1 C8 144.2(5) . . ? C5 Mo1 C8 118.2(7) . . ? C4 Mo1 C8 72.0(6) . . ? C2 Mo1 C7 112.0(9) . . ? C3 Mo1 C7 74.1(8) . . ? C1 Mo1 C7 73.8(5) . . ? C5 Mo1 C7 142.2(8) . . ? C4 Mo1 C7 144.2(7) . . ? C8 Mo1 C7 78.3(5) . . ? C2 Mo1 C6 144.5(9) . . ? C3 Mo1 C6 140.6(7) . . ? C1 Mo1 C6 77.9(5) . . ? C5 Mo1 C6 75.9(8) . . ? C4 Mo1 C6 112.5(7) . . ? C8 Mo1 C6 74.2(5) . . ? C7 Mo1 C6 77.0(7) . . ? C9 N1 C11 121(2) . . ? C9 N1 C10 120.4(18) . . ? C11 N1 C10 117(2) . . ? C12 N2 C13 120.6(17) . . ? C12 N2 C14 116.0(19) . . ? C13 N2 C14 123.2(17) . . ? C20 N3 C18 122(3) . . ? C20 N3 C19 120(2) . . ? C18 N3 C19 118(3) . . ? C23 N4 C21 121(3) . . ? C23 N4 C22 121(3) . . ? C21 N4 C22 118(3) . . ? C8 N5 Er1 175.3(13) . . ? C1 N10 Er1 174.3(11) . 1_565 ? C17 N13 C16 122(2) . . ? C17 N13 C15 112(3) . . ? C16 N13 C15 125(3) . . ? C24 N14 C25 130(3) . . ? C24 N14 C26 124(2) . . ? C25 N14 C26 100(2) . . ? C12 O1 Er1 132.2(12) . . ? C9 O2 Er1 140.9(11) . . ? C24 O3 Er1 153.3(18) . . ? C23 O4 Er1 145(2) . . ? C20 O5 Er1 141.2(17) . . ? C17 O6 Er1 130.3(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N9 C2 Mo1 C3 -15(34) . . . . ? N9 C2 Mo1 C1 113(35) . . . . ? N9 C2 Mo1 C5 -169(35) . . . . ? N9 C2 Mo1 C4 -96(35) . . . . ? N9 C2 Mo1 C8 -49(35) . . . . ? N9 C2 Mo1 C7 49(35) . . . . ? N9 C2 Mo1 C6 148(34) . . . . ? N11 C3 Mo1 C2 82(28) . . . . ? N11 C3 Mo1 C1 24(29) . . . . ? N11 C3 Mo1 C5 125(28) . . . . ? N11 C3 Mo1 C4 166(29) . . . . ? N11 C3 Mo1 C8 -120(29) . . . . ? N11 C3 Mo1 C7 -37(28) . . . . ? N11 C3 Mo1 C6 -82(29) . . . . ? N10 C1 Mo1 C2 79(20) . . . . ? N10 C1 Mo1 C3 137(20) . . . . ? N10 C1 Mo1 C5 -3(20) . . . . ? N10 C1 Mo1 C4 30(20) . . . . ? N10 C1 Mo1 C8 -121(20) . . . . ? N10 C1 Mo1 C7 -161(20) . . . . ? N10 C1 Mo1 C6 -81(20) . . . . ? N8 C5 Mo1 C2 -112(24) . . . . ? N8 C5 Mo1 C3 -153(23) . . . . ? N8 C5 Mo1 C1 -37(24) . . . . ? N8 C5 Mo1 C4 164(24) . . . . ? N8 C5 Mo1 C8 107(24) . . . . ? N8 C5 Mo1 C7 -1(25) . . . . ? N8 C5 Mo1 C6 44(24) . . . . ? N7 C4 Mo1 C2 -35(75) . . . . ? N7 C4 Mo1 C3 -109(75) . . . . ? N7 C4 Mo1 C1 12(76) . . . . ? N7 C4 Mo1 C5 45(75) . . . . ? N7 C4 Mo1 C8 174(100) . . . . ? N7 C4 Mo1 C7 -150(75) . . . . ? N7 C4 Mo1 C6 111(75) . . . . ? N5 C8 Mo1 C2 34(37) . . . . ? N5 C8 Mo1 C3 0(37) . . . . ? N5 C8 Mo1 C1 -116(36) . . . . ? N5 C8 Mo1 C5 139(37) . . . . ? N5 C8 Mo1 C4 83(37) . . . . ? N5 C8 Mo1 C7 -77(37) . . . . ? N5 C8 Mo1 C6 -157(37) . . . . ? N12 C7 Mo1 C2 148(83) . . . . ? N12 C7 Mo1 C3 -149(83) . . . . ? N12 C7 Mo1 C1 85(83) . . . . ? N12 C7 Mo1 C5 49(83) . . . . ? N12 C7 Mo1 C4 -106(83) . . . . ? N12 C7 Mo1 C8 -72(83) . . . . ? N12 C7 Mo1 C6 4(83) . . . . ? N6 C6 Mo1 C2 -56(19) . . . . ? N6 C6 Mo1 C3 98(19) . . . . ? N6 C6 Mo1 C1 -22(19) . . . . ? N6 C6 Mo1 C5 -99(19) . . . . ? N6 C6 Mo1 C4 -162(19) . . . . ? N6 C6 Mo1 C8 136(19) . . . . ? N6 C6 Mo1 C7 54(19) . . . . ? O2 C9 N1 C11 174(2) . . . . ? O2 C9 N1 C10 8(4) . . . . ? O1 C12 N2 C13 1(3) . . . . ? O1 C12 N2 C14 176.7(18) . . . . ? O5 C20 N3 C18 -174(3) . . . . ? O5 C20 N3 C19 0(4) . . . . ? O4 C23 N4 C21 -19(6) . . . . ? O4 C23 N4 C22 166(4) . . . . ? Mo1 C8 N5 Er1 12(48) . . . . ? O3 Er1 N5 C8 -35(13) . . . . ? O4 Er1 N5 C8 39(13) . . . . ? O2 Er1 N5 C8 -121(13) . . . . ? O5 Er1 N5 C8 119(13) . . . . ? O1 Er1 N5 C8 177(100) . . . . ? O6 Er1 N5 C8 77(13) . . . . ? N10 Er1 N5 C8 -75(13) 1_545 . . . ? Mo1 C1 N10 Er1 96(22) . . . 1_565 ? O6 C17 N13 C16 -179(3) . . . . ? O6 C17 N13 C15 9(5) . . . . ? O3 C24 N14 C25 56(5) . . . . ? O3 C24 N14 C26 -158(3) . . . . ? N2 C12 O1 Er1 -178.1(15) . . . . ? O3 Er1 O1 C12 -12(2) . . . . ? O4 Er1 O1 C12 -155.0(16) . . . . ? O2 Er1 O1 C12 39.1(17) . . . . ? O5 Er1 O1 C12 157.6(18) . . . . ? O6 Er1 O1 C12 -120.8(17) . . . . ? N10 Er1 O1 C12 -42.4(17) 1_545 . . . ? N5 Er1 O1 C12 101.5(17) . . . . ? N1 C9 O2 Er1 -173.1(16) . . . . ? O3 Er1 O2 C9 -56(2) . . . . ? O4 Er1 O2 C9 -13(3) . . . . ? O5 Er1 O2 C9 85(2) . . . . ? O1 Er1 O2 C9 150(2) . . . . ? O6 Er1 O2 C9 -177.1(19) . . . . ? N10 Er1 O2 C9 -131(2) 1_545 . . . ? N5 Er1 O2 C9 22(2) . . . . ? N14 C24 O3 Er1 167(2) . . . . ? O4 Er1 O3 C24 -71(4) . . . . ? O2 Er1 O3 C24 85(4) . . . . ? O5 Er1 O3 C24 -30(5) . . . . ? O1 Er1 O3 C24 133(4) . . . . ? O6 Er1 O3 C24 -131(4) . . . . ? N10 Er1 O3 C24 164(5) 1_545 . . . ? N5 Er1 O3 C24 8(4) . . . . ? N4 C23 O4 Er1 157(3) . . . . ? O3 Er1 O4 C23 67(4) . . . . ? O2 Er1 O4 C23 22(5) . . . . ? O5 Er1 O4 C23 -87(4) . . . . ? O1 Er1 O4 C23 -134(4) . . . . ? O6 Er1 O4 C23 -169(4) . . . . ? N10 Er1 O4 C23 128(4) 1_545 . . . ? N5 Er1 O4 C23 -14(4) . . . . ? N3 C20 O5 Er1 167.9(19) . . . . ? O3 Er1 O5 C20 -153(3) . . . . ? O4 Er1 O5 C20 -113(3) . . . . ? O2 Er1 O5 C20 102(3) . . . . ? O1 Er1 O5 C20 37(3) . . . . ? O6 Er1 O5 C20 -39(3) . . . . ? N10 Er1 O5 C20 2(3) 1_545 . . . ? N5 Er1 O5 C20 167(3) . . . . ? N13 C17 O6 Er1 -168(2) . . . . ? O3 Er1 O6 C17 -104(2) . . . . ? O4 Er1 O6 C17 -164(2) . . . . ? O2 Er1 O6 C17 7(3) . . . . ? O5 Er1 O6 C17 117(2) . . . . ? O1 Er1 O6 C17 39(2) . . . . ? N10 Er1 O6 C17 -40(2) 1_545 . . . ? N5 Er1 O6 C17 157(2) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.023 _refine_diff_density_min -1.938 _refine_diff_density_rms 0.219 _database_code_depnum_ccdc_archive 'CCDC 869790' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl3 #TrackingRef 'shelxl-Tm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H42 Mo N14 O6 Tm' _chemical_formula_weight 911.61 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' Mo Mo -1.6832 0.6857 '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' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.405(3) _cell_length_b 10.957(2) _cell_length_c 21.382(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.21(3) _cell_angle_gamma 90.00 _cell_volume 3842.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.24 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1819 _exptl_absorpt_coefficient_mu 2.675 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5907 _exptl_absorpt_correction_T_max 0.7396 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26139 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6777 _reflns_number_gt 5618 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+16.0280P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6777 _refine_ls_number_parameters 445 _refine_ls_number_restraints 109 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.1824 _refine_ls_wR_factor_gt 0.1652 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_restrained_S_all 1.212 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_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_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 C1 C 0.3328(8) -0.2717(10) 0.2185(6) 0.054(3) Uani 1 1 d . . . C2 C 0.1682(7) -0.2700(10) 0.2170(6) 0.049(3) Uani 1 1 d . . . C3 C 0.2579(6) -0.0857(10) 0.1672(5) 0.038(2) Uani 1 1 d . . . C4 C 0.1385(8) -0.1915(11) 0.1020(6) 0.059(3) Uani 1 1 d . . . C5 C 0.2952(9) -0.1718(12) 0.0600(6) 0.062(3) Uani 1 1 d . . . C6 C 0.2049(8) -0.3873(11) 0.0613(6) 0.055(3) Uani 1 1 d . . . C7 C 0.3607(8) -0.3580(11) 0.1075(6) 0.057(3) Uani 1 1 d . . . C8 C 0.2416(6) -0.4606(9) 0.1720(4) 0.035(2) Uani 1 1 d . . . C9 C 0.2846(9) 0.0056(12) 0.3245(6) 0.070(4) Uani 1 1 d . . . H9 H 0.2535 -0.0435 0.2977 0.084 Uiso 1 1 calc R . . C10 C 0.1960(9) 0.3325(14) 0.3597(8) 0.076(4) Uani 1 1 d . . . H10 H 0.1801 0.2557 0.3734 0.091 Uiso 1 1 calc R . . C11 C 0.1232(7) 0.2857(10) 0.1005(5) 0.049(3) Uani 1 1 d . . . H11 H 0.1557 0.3501 0.0875 0.059 Uiso 1 1 calc R . . C12 C 0.0879(7) 0.0561(10) 0.2427(6) 0.048(3) Uani 1 1 d . . . H12 H 0.0943 0.0301 0.2017 0.057 Uiso 1 1 calc R . . C13 C 0.0262(10) 0.3418(14) 0.0180(8) 0.097(6) Uani 1 1 d . . . H13A H 0.0683 0.3981 0.0069 0.146 Uiso 1 1 calc R . . H13B H -0.0212 0.3864 0.0303 0.146 Uiso 1 1 calc R . . H13C H 0.0126 0.2914 -0.0174 0.146 Uiso 1 1 calc R . . C14 C -0.0006(9) 0.1677(16) 0.0884(9) 0.101(6) Uani 1 1 d . . . H14A H 0.0300 0.0945 0.0966 0.152 Uiso 1 1 calc R . . H14B H -0.0397 0.1530 0.0552 0.152 Uiso 1 1 calc R . . H14C H -0.0284 0.1917 0.1255 0.152 Uiso 1 1 calc R . . C15 C -0.0316(8) -0.0723(13) 0.2450(8) 0.082(5) Uani 1 1 d . . . H15A H -0.0179 -0.0839 0.2020 0.122 Uiso 1 1 calc R . . H15B H -0.0858 -0.0397 0.2472 0.122 Uiso 1 1 calc R . . H15C H -0.0290 -0.1491 0.2665 0.122 Uiso 1 1 calc R . . C16 C 0.0135(10) 0.0517(17) 0.3388(8) 0.096(5) Uani 1 1 d . . . H16A H 0.0422 -0.0024 0.3668 0.145 Uiso 1 1 calc R . . H16B H -0.0437 0.0495 0.3474 0.145 Uiso 1 1 calc R . . H16C H 0.0336 0.1333 0.3445 0.145 Uiso 1 1 calc R . . C17 C 0.3508(17) 0.034(2) 0.4238(10) 0.173(12) Uani 1 1 d . . . H17A H 0.3978 0.0694 0.4048 0.260 Uiso 1 1 calc R . . H17B H 0.3679 -0.0152 0.4588 0.260 Uiso 1 1 calc R . . H17C H 0.3157 0.0981 0.4380 0.260 Uiso 1 1 calc R . . C18 C 0.2824(13) -0.1620(16) 0.3954(9) 0.118(7) Uani 1 1 d . . . H18A H 0.2502 -0.1579 0.4322 0.177 Uiso 1 1 calc R . . H18B H 0.3300 -0.2108 0.4037 0.177 Uiso 1 1 calc R . . H18C H 0.2509 -0.1981 0.3619 0.177 Uiso 1 1 calc R . . C19 C 0.1638(16) 0.406(2) 0.4629(9) 0.150(10) Uani 1 1 d . . . H19A H 0.1058 0.4178 0.4620 0.225 Uiso 1 1 calc R . . H19B H 0.1890 0.4647 0.4903 0.225 Uiso 1 1 calc R . . H19C H 0.1760 0.3250 0.4777 0.225 Uiso 1 1 calc R . . C20 C 0.2176(13) 0.5387(14) 0.3840(8) 0.109(7) Uani 1 1 d . . . H20A H 0.2716 0.5377 0.3675 0.164 Uiso 1 1 calc R . . H20B H 0.2168 0.5896 0.4205 0.164 Uiso 1 1 calc R . . H20C H 0.1800 0.5702 0.3529 0.164 Uiso 1 1 calc R . . C21 C 0.3556(13) 0.1964(19) 0.0928(10) 0.111(4) Uani 1 1 d U . . H21 H 0.3354 0.1189 0.0837 0.134 Uiso 1 1 calc R . . C22 C 0.4254(17) 0.141(3) 0.0088(13) 0.179(8) Uani 1 1 d U . . H22A H 0.3941 0.1600 -0.0284 0.268 Uiso 1 1 calc R . . H22B H 0.4090 0.0628 0.0244 0.268 Uiso 1 1 calc R . . H22C H 0.4823 0.1389 -0.0008 0.268 Uiso 1 1 calc R . . C23 C 0.4740(16) 0.315(2) 0.0567(14) 0.195(9) Uani 1 1 d DU . . H23A H 0.4614 0.3727 0.0887 0.292 Uiso 1 1 calc R . . H23B H 0.4781 0.3559 0.0173 0.292 Uiso 1 1 calc R . . H23C H 0.5248 0.2755 0.0670 0.292 Uiso 1 1 calc R . . C24 C 0.5206(13) 0.521(2) 0.2553(10) 0.133(7) Uani 1 1 d U . . H24A H 0.4986 0.5435 0.2149 0.200 Uiso 1 1 calc R . . H24B H 0.5742 0.4877 0.2508 0.200 Uiso 1 1 calc R . . H24C H 0.5237 0.5926 0.2814 0.200 Uiso 1 1 calc R . . C25 C 0.4875(14) 0.408(2) 0.3443(11) 0.149(7) Uani 1 1 d U . . H25A H 0.4588 0.4637 0.3706 0.223 Uiso 1 1 calc R . . H25B H 0.5451 0.4168 0.3516 0.223 Uiso 1 1 calc R . . H25C H 0.4715 0.3259 0.3537 0.223 Uiso 1 1 calc R . . C26 C 0.4150(10) 0.3856(16) 0.2473(9) 0.090(3) Uani 1 1 d U . . H26 H 0.4082 0.4269 0.2095 0.108 Uiso 1 1 calc R . . Mo1 Mo 0.24982(6) -0.27461(8) 0.13834(4) 0.0361(2) Uani 1 1 d . . . N1 N 0.3202(10) -0.1177(12) 0.0190(6) 0.097(5) Uani 1 1 d . . . N2 N 0.3736(8) -0.2677(11) 0.2629(6) 0.079(4) Uani 1 1 d . . . N3 N 0.4206(8) -0.3985(14) 0.0923(7) 0.099(4) Uani 1 1 d . . . N4 N 0.2390(5) -0.5599(8) 0.1866(4) 0.040(2) Uani 1 1 d . . . N5 N 0.1816(8) -0.4470(10) 0.0210(5) 0.079(4) Uani 1 1 d . . . N6 N 0.1285(8) -0.2658(10) 0.2611(6) 0.073(3) Uani 1 1 d . . . N7 N 0.0791(8) -0.1451(12) 0.0864(6) 0.086(4) Uani 1 1 d . . . N8 N 0.2603(5) 0.0141(7) 0.1821(4) 0.040(2) Uani 1 1 d . . . N9 N 0.3066(8) -0.0420(10) 0.3779(5) 0.073(3) Uani 1 1 d . . . N10 N 0.1950(7) 0.4207(11) 0.3999(5) 0.071(3) Uani 1 1 d . . . N11 N 0.0550(6) 0.2650(9) 0.0699(5) 0.057(3) Uani 1 1 d . . . N12 N 0.0262(6) 0.0132(9) 0.2744(5) 0.056(3) Uani 1 1 d . . . N13 N 0.4124(11) 0.2274(16) 0.0526(8) 0.113(4) Uani 1 1 d DU . . N14 N 0.4690(7) 0.4331(12) 0.2832(6) 0.079(3) Uani 1 1 d U . . O1 O 0.1378(4) 0.1300(7) 0.2652(3) 0.0494(19) Uani 1 1 d . . . O2 O 0.1471(5) 0.2248(6) 0.1457(4) 0.0481(19) Uani 1 1 d . . . O3 O 0.2162(5) 0.3419(7) 0.3049(4) 0.058(2) Uani 1 1 d . . . O4 O 0.3005(5) 0.1084(7) 0.3059(4) 0.054(2) Uani 1 1 d . . . O5 O 0.3741(6) 0.3047(8) 0.2515(5) 0.078(3) Uani 1 1 d U . . O6 O 0.3263(6) 0.2333(9) 0.1320(5) 0.078(3) Uani 1 1 d U . . Tm1 Tm 0.25092(3) 0.22364(4) 0.22148(2) 0.03412(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.063(8) 0.037(6) 0.062(8) -0.009(6) -0.003(6) 0.006(6) C2 0.046(7) 0.040(6) 0.061(8) 0.004(6) -0.001(6) 0.011(5) C3 0.041(6) 0.032(6) 0.042(6) 0.007(5) 0.003(4) -0.004(5) C4 0.058(8) 0.047(7) 0.072(8) -0.009(6) -0.026(6) 0.011(6) C5 0.097(10) 0.040(7) 0.049(7) 0.004(6) 0.001(7) 0.004(7) C6 0.074(9) 0.039(7) 0.050(7) 0.003(6) -0.002(6) -0.008(6) C7 0.064(8) 0.051(8) 0.058(8) 0.004(6) 0.020(6) 0.000(6) C8 0.044(6) 0.026(6) 0.036(5) -0.001(4) 0.001(4) -0.003(4) C9 0.093(11) 0.050(9) 0.068(9) 0.013(7) 0.014(7) 0.022(7) C10 0.086(11) 0.054(9) 0.089(12) 0.013(8) 0.009(8) -0.017(8) C11 0.060(7) 0.034(6) 0.052(7) 0.008(5) -0.016(6) -0.009(5) C12 0.043(6) 0.043(7) 0.058(7) 0.008(5) 0.008(5) -0.004(5) C13 0.115(13) 0.070(10) 0.104(12) 0.026(9) -0.066(11) -0.006(10) C14 0.066(10) 0.106(14) 0.130(15) 0.007(12) -0.026(10) -0.034(10) C15 0.042(7) 0.063(9) 0.140(14) 0.001(9) 0.014(8) -0.019(7) C16 0.079(11) 0.116(14) 0.096(12) -0.005(11) 0.042(9) -0.018(10) C17 0.24(3) 0.16(2) 0.118(18) 0.044(16) -0.071(19) -0.09(2) C18 0.18(2) 0.076(12) 0.095(13) 0.029(11) 0.015(13) 0.001(13) C19 0.23(3) 0.124(19) 0.095(15) -0.010(14) 0.052(16) -0.031(18) C20 0.17(2) 0.051(10) 0.102(14) 0.017(9) -0.018(13) -0.014(11) C21 0.113(7) 0.112(6) 0.110(7) 0.000(6) 0.028(6) -0.004(6) C22 0.185(11) 0.172(11) 0.180(11) -0.010(9) 0.015(9) 0.003(9) C23 0.195(12) 0.189(12) 0.200(12) -0.006(9) 0.009(9) -0.005(9) C24 0.120(9) 0.128(10) 0.152(10) 0.017(8) 0.009(8) 0.012(8) C25 0.143(10) 0.163(10) 0.140(10) -0.001(8) -0.001(8) 0.005(8) C26 0.073(6) 0.084(6) 0.113(6) -0.007(6) -0.013(5) -0.016(5) Mo1 0.0491(5) 0.0192(4) 0.0399(5) -0.0006(4) 0.0002(4) 0.0000(4) N1 0.168(14) 0.066(8) 0.057(8) 0.019(7) 0.024(8) -0.017(9) N2 0.081(8) 0.080(9) 0.073(8) -0.017(6) -0.037(7) 0.016(7) N3 0.076(9) 0.113(12) 0.109(11) 0.013(9) 0.033(8) 0.023(8) N4 0.051(5) 0.026(5) 0.044(5) 0.003(4) 0.003(4) -0.006(4) N5 0.130(11) 0.052(7) 0.055(7) -0.010(6) -0.015(7) -0.030(7) N6 0.081(8) 0.060(7) 0.078(8) 0.003(6) 0.029(7) 0.014(6) N7 0.085(9) 0.077(9) 0.094(9) -0.006(7) -0.035(7) 0.018(7) N8 0.042(5) 0.017(5) 0.059(6) -0.001(4) 0.003(4) -0.002(4) N9 0.108(9) 0.054(7) 0.057(7) 0.024(6) -0.006(6) -0.006(6) N10 0.093(9) 0.071(8) 0.050(6) -0.020(6) 0.010(6) -0.006(6) N11 0.058(6) 0.044(6) 0.069(7) -0.002(5) -0.025(5) 0.005(5) N12 0.048(6) 0.046(6) 0.074(7) 0.005(5) 0.011(5) -0.007(5) N13 0.117(7) 0.118(7) 0.106(7) -0.012(6) 0.042(6) -0.014(6) N14 0.058(5) 0.082(6) 0.095(6) -0.002(5) -0.013(5) -0.015(5) O1 0.044(4) 0.049(5) 0.056(5) 0.000(4) 0.013(3) -0.015(4) O2 0.049(5) 0.037(4) 0.058(5) 0.008(4) -0.014(4) -0.007(3) O3 0.083(6) 0.043(5) 0.049(5) -0.008(4) 0.005(4) 0.002(4) O4 0.067(5) 0.033(4) 0.060(5) 0.021(4) -0.013(4) -0.004(4) O5 0.058(5) 0.058(5) 0.118(6) 0.013(5) -0.018(4) -0.026(4) O6 0.085(5) 0.060(5) 0.090(6) -0.010(4) 0.053(5) 0.005(4) Tm1 0.0345(3) 0.0209(3) 0.0471(3) 0.00069(19) 0.00133(18) -0.00252(18) _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 C1 N2 1.152(15) . ? C1 Mo1 2.166(13) . ? C2 N6 1.157(16) . ? C2 Mo1 2.173(13) . ? C3 N8 1.139(12) . ? C3 Mo1 2.163(11) . ? C4 N7 1.142(15) . ? C4 Mo1 2.170(12) . ? C5 N1 1.141(16) . ? C5 Mo1 2.164(13) . ? C6 N5 1.142(14) . ? C6 Mo1 2.175(12) . ? C7 N3 1.131(16) . ? C7 Mo1 2.152(13) . ? C8 N4 1.134(12) . ? C8 Mo1 2.166(10) . ? C9 O4 1.225(15) . ? C9 N9 1.298(15) . ? C9 H9 0.9300 . ? C10 O3 1.228(16) . ? C10 N10 1.294(18) . ? C10 H10 0.9300 . ? C11 O2 1.231(12) . ? C11 N11 1.304(14) . ? C11 H11 0.9300 . ? C12 O1 1.241(12) . ? C12 N12 1.317(14) . ? C12 H12 0.9300 . ? C13 N11 1.464(15) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N11 1.463(18) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N12 1.465(16) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N12 1.459(18) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N9 1.47(2) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N9 1.425(19) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N10 1.46(2) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N10 1.389(18) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 O6 1.06(2) . ? C21 N13 1.32(2) . ? C21 H21 0.9300 . ? C22 N13 1.35(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 N13 1.393(10) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N14 1.42(2) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N14 1.36(2) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O5 1.117(17) . ? C26 N14 1.272(17) . ? C26 H26 0.9300 . ? N4 Tm1 2.492(9) 1_545 ? N8 Tm1 2.452(8) . ? O1 Tm1 2.333(7) . ? O2 Tm1 2.326(7) . ? O3 Tm1 2.286(8) . ? O4 Tm1 2.335(7) . ? O5 Tm1 2.286(8) . ? O6 Tm1 2.302(9) . ? Tm1 N4 2.493(9) 1_565 ? 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 N2 C1 Mo1 176.4(12) . . ? N6 C2 Mo1 176.1(12) . . ? N8 C3 Mo1 178.4(9) . . ? N7 C4 Mo1 175.9(12) . . ? N1 C5 Mo1 179.0(14) . . ? N5 C6 Mo1 179.6(13) . . ? N3 C7 Mo1 177.5(14) . . ? N4 C8 Mo1 176.2(9) . . ? O4 C9 N9 126.7(15) . . ? O4 C9 H9 116.6 . . ? N9 C9 H9 116.6 . . ? O3 C10 N10 125.4(14) . . ? O3 C10 H10 117.3 . . ? N10 C10 H10 117.3 . . ? O2 C11 N11 123.7(11) . . ? O2 C11 H11 118.2 . . ? N11 C11 H11 118.2 . . ? O1 C12 N12 122.8(11) . . ? O1 C12 H12 118.6 . . ? N12 C12 H12 118.6 . . ? N11 C13 H13A 109.5 . . ? N11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N11 C14 H14A 109.5 . . ? N11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N12 C15 H15A 109.5 . . ? N12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N12 C16 H16A 109.5 . . ? N12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N9 C17 H17A 109.5 . . ? N9 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N9 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N9 C18 H18A 109.5 . . ? N9 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N9 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N10 C19 H19A 109.5 . . ? N10 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N10 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N10 C20 H20A 109.5 . . ? N10 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N10 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O6 C21 N13 139(2) . . ? O6 C21 H21 110.5 . . ? N13 C21 H21 110.5 . . ? N13 C22 H22A 109.5 . . ? N13 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N13 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N13 C23 H23A 109.5 . . ? N13 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N13 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N14 C24 H24A 109.5 . . ? N14 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N14 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N14 C25 H25A 109.5 . . ? N14 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N14 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O5 C26 N14 133.5(19) . . ? O5 C26 H26 113.2 . . ? N14 C26 H26 113.2 . . ? C7 Mo1 C3 116.5(4) . . ? C7 Mo1 C5 71.1(5) . . ? C3 Mo1 C5 72.7(4) . . ? C7 Mo1 C8 76.2(4) . . ? C3 Mo1 C8 144.0(4) . . ? C5 Mo1 C8 140.5(4) . . ? C7 Mo1 C1 74.2(5) . . ? C3 Mo1 C1 74.1(4) . . ? C5 Mo1 C1 112.6(5) . . ? C8 Mo1 C1 78.1(4) . . ? C7 Mo1 C4 141.2(5) . . ? C3 Mo1 C4 75.3(4) . . ? C5 Mo1 C4 78.8(5) . . ? C8 Mo1 C4 117.1(4) . . ? C1 Mo1 C4 141.9(5) . . ? C7 Mo1 C2 141.8(4) . . ? C3 Mo1 C2 78.0(4) . . ? C5 Mo1 C2 144.6(4) . . ? C8 Mo1 C2 73.8(4) . . ? C1 Mo1 C2 76.9(5) . . ? C4 Mo1 C2 74.9(5) . . ? C7 Mo1 C6 78.6(5) . . ? C3 Mo1 C6 141.0(4) . . ? C5 Mo1 C6 80.0(5) . . ? C8 Mo1 C6 72.2(4) . . ? C1 Mo1 C6 143.6(4) . . ? C4 Mo1 C6 72.4(5) . . ? C2 Mo1 C6 113.3(5) . . ? C8 N4 Tm1 173.2(8) . 1_545 ? C3 N8 Tm1 173.1(8) . . ? C9 N9 C18 121.8(14) . . ? C9 N9 C17 118.9(13) . . ? C18 N9 C17 119.0(13) . . ? C10 N10 C20 121.7(14) . . ? C10 N10 C19 122.6(15) . . ? C20 N10 C19 115.5(14) . . ? C11 N11 C14 121.6(11) . . ? C11 N11 C13 122.7(11) . . ? C14 N11 C13 115.5(11) . . ? C12 N12 C16 120.6(11) . . ? C12 N12 C15 120.3(12) . . ? C16 N12 C15 119.1(11) . . ? C21 N13 C22 113(2) . . ? C21 N13 C23 131(2) . . ? C22 N13 C23 114(2) . . ? C26 N14 C25 129.3(17) . . ? C26 N14 C24 115.9(16) . . ? C25 N14 C24 114.6(16) . . ? C12 O1 Tm1 131.0(7) . . ? C11 O2 Tm1 140.0(7) . . ? C10 O3 Tm1 140.7(9) . . ? C9 O4 Tm1 132.5(9) . . ? C26 O5 Tm1 144.6(11) . . ? C21 O6 Tm1 154.6(15) . . ? O5 Tm1 O3 78.1(4) . . ? O5 Tm1 O6 74.2(4) . . ? O3 Tm1 O6 140.3(3) . . ? O5 Tm1 O2 145.4(3) . . ? O3 Tm1 O2 110.5(3) . . ? O6 Tm1 O2 79.6(4) . . ? O5 Tm1 O1 139.8(3) . . ? O3 Tm1 O1 73.9(3) . . ? O6 Tm1 O1 143.0(3) . . ? O2 Tm1 O1 72.8(3) . . ? O5 Tm1 O4 72.6(3) . . ? O3 Tm1 O4 78.0(3) . . ? O6 Tm1 O4 118.8(4) . . ? O2 Tm1 O4 141.2(3) . . ? O1 Tm1 O4 73.7(3) . . ? O5 Tm1 N8 113.5(3) . . ? O3 Tm1 N8 144.8(3) . . ? O6 Tm1 N8 73.7(3) . . ? O2 Tm1 N8 79.4(3) . . ? O1 Tm1 N8 77.4(3) . . ? O4 Tm1 N8 74.7(3) . . ? O5 Tm1 N4 77.2(3) . 1_565 ? O3 Tm1 N4 71.0(3) . 1_565 ? O6 Tm1 N4 75.4(3) . 1_565 ? O2 Tm1 N4 74.6(3) . 1_565 ? O1 Tm1 N4 118.7(3) . 1_565 ? O4 Tm1 N4 140.3(3) . 1_565 ? N8 Tm1 N4 142.5(3) . 1_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C7 Mo1 C3 19(30) . . . . ? N3 C7 Mo1 C5 77(29) . . . . ? N3 C7 Mo1 C8 -125(30) . . . . ? N3 C7 Mo1 C1 -44(29) . . . . ? N3 C7 Mo1 C4 118(29) . . . . ? N3 C7 Mo1 C2 -86(30) . . . . ? N3 C7 Mo1 C6 160(30) . . . . ? N8 C3 Mo1 C7 154(34) . . . . ? N8 C3 Mo1 C5 96(34) . . . . ? N8 C3 Mo1 C8 -102(34) . . . . ? N8 C3 Mo1 C1 -143(34) . . . . ? N8 C3 Mo1 C4 14(34) . . . . ? N8 C3 Mo1 C2 -64(34) . . . . ? N8 C3 Mo1 C6 49(34) . . . . ? N1 C5 Mo1 C7 -45(77) . . . . ? N1 C5 Mo1 C3 81(77) . . . . ? N1 C5 Mo1 C8 -81(77) . . . . ? N1 C5 Mo1 C1 18(77) . . . . ? N1 C5 Mo1 C4 159(77) . . . . ? N1 C5 Mo1 C2 117(77) . . . . ? N1 C5 Mo1 C6 -127(77) . . . . ? N4 C8 Mo1 C7 -40(14) . . . . ? N4 C8 Mo1 C3 -157(13) . . . . ? N4 C8 Mo1 C5 -6(14) . . . . ? N4 C8 Mo1 C1 -117(14) . . . . ? N4 C8 Mo1 C4 100(14) . . . . ? N4 C8 Mo1 C2 163(14) . . . . ? N4 C8 Mo1 C6 42(14) . . . . ? N2 C1 Mo1 C7 -176(19) . . . . ? N2 C1 Mo1 C3 60(19) . . . . ? N2 C1 Mo1 C5 123(19) . . . . ? N2 C1 Mo1 C8 -97(19) . . . . ? N2 C1 Mo1 C4 22(20) . . . . ? N2 C1 Mo1 C2 -21(19) . . . . ? N2 C1 Mo1 C6 -133(19) . . . . ? N7 C4 Mo1 C7 -166(18) . . . . ? N7 C4 Mo1 C3 -52(18) . . . . ? N7 C4 Mo1 C5 -127(18) . . . . ? N7 C4 Mo1 C8 92(18) . . . . ? N7 C4 Mo1 C1 -14(19) . . . . ? N7 C4 Mo1 C2 29(18) . . . . ? N7 C4 Mo1 C6 150(18) . . . . ? N6 C2 Mo1 C7 55(16) . . . . ? N6 C2 Mo1 C3 -63(16) . . . . ? N6 C2 Mo1 C5 -97(16) . . . . ? N6 C2 Mo1 C8 95(16) . . . . ? N6 C2 Mo1 C1 14(16) . . . . ? N6 C2 Mo1 C4 -140(16) . . . . ? N6 C2 Mo1 C6 157(16) . . . . ? N5 C6 Mo1 C7 40(100) . . . . ? N5 C6 Mo1 C3 158(100) . . . . ? N5 C6 Mo1 C5 112(100) . . . . ? N5 C6 Mo1 C8 -39(100) . . . . ? N5 C6 Mo1 C1 -2(100) . . . . ? N5 C6 Mo1 C4 -166(100) . . . . ? N5 C6 Mo1 C2 -102(100) . . . . ? Mo1 C8 N4 Tm1 79(16) . . . 1_545 ? Mo1 C3 N8 Tm1 50(38) . . . . ? O4 C9 N9 C18 178.2(15) . . . . ? O4 C9 N9 C17 4(3) . . . . ? O3 C10 N10 C20 0(3) . . . . ? O3 C10 N10 C19 174.7(18) . . . . ? O2 C11 N11 C14 2(2) . . . . ? O2 C11 N11 C13 177.4(14) . . . . ? O1 C12 N12 C16 0.2(18) . . . . ? O1 C12 N12 C15 179.0(11) . . . . ? O6 C21 N13 C22 -179(3) . . . . ? O6 C21 N13 C23 20(5) . . . . ? O5 C26 N14 C25 -10(4) . . . . ? O5 C26 N14 C24 167(2) . . . . ? N12 C12 O1 Tm1 -179.1(8) . . . . ? N11 C11 O2 Tm1 -173.5(9) . . . . ? N10 C10 O3 Tm1 165.6(10) . . . . ? N9 C9 O4 Tm1 -168.0(10) . . . . ? N14 C26 O5 Tm1 151.0(16) . . . . ? N13 C21 O6 Tm1 -161(2) . . . . ? C26 O5 Tm1 O3 -84(2) . . . . ? C26 O5 Tm1 O6 67(2) . . . . ? C26 O5 Tm1 O2 25(3) . . . . ? C26 O5 Tm1 O1 -131(2) . . . . ? C26 O5 Tm1 O4 -165(2) . . . . ? C26 O5 Tm1 N8 131(2) . . . . ? C26 O5 Tm1 N4 -11(2) . . . 1_565 ? C10 O3 Tm1 O5 -106.7(15) . . . . ? C10 O3 Tm1 O6 -153.2(14) . . . . ? C10 O3 Tm1 O2 108.3(15) . . . . ? C10 O3 Tm1 O1 44.1(14) . . . . ? C10 O3 Tm1 O4 -32.2(14) . . . . ? C10 O3 Tm1 N8 7.5(17) . . . . ? C10 O3 Tm1 N4 173.0(15) . . . 1_565 ? C21 O6 Tm1 O5 120(4) . . . . ? C21 O6 Tm1 O3 167(3) . . . . ? C21 O6 Tm1 O2 -83(4) . . . . ? C21 O6 Tm1 O1 -41(4) . . . . ? C21 O6 Tm1 O4 60(4) . . . . ? C21 O6 Tm1 N8 -1(4) . . . . ? C21 O6 Tm1 N4 -160(4) . . . 1_565 ? C11 O2 Tm1 O5 -13.0(15) . . . . ? C11 O2 Tm1 O3 85.9(13) . . . . ? C11 O2 Tm1 O6 -54.1(13) . . . . ? C11 O2 Tm1 O1 150.8(13) . . . . ? C11 O2 Tm1 O4 -177.8(11) . . . . ? C11 O2 Tm1 N8 -129.3(13) . . . . ? C11 O2 Tm1 N4 23.4(12) . . . 1_565 ? C12 O1 Tm1 O5 -152.8(9) . . . . ? C12 O1 Tm1 O3 159.5(10) . . . . ? C12 O1 Tm1 O6 -2.1(12) . . . . ? C12 O1 Tm1 O2 41.5(9) . . . . ? C12 O1 Tm1 O4 -118.6(10) . . . . ? C12 O1 Tm1 N8 -41.2(9) . . . . ? C12 O1 Tm1 N4 102.4(10) . . . 1_565 ? C9 O4 Tm1 O5 -159.9(12) . . . . ? C9 O4 Tm1 O3 118.9(12) . . . . ? C9 O4 Tm1 O6 -99.7(12) . . . . ? C9 O4 Tm1 O2 11.1(14) . . . . ? C9 O4 Tm1 O1 42.4(12) . . . . ? C9 O4 Tm1 N8 -38.7(12) . . . . ? C9 O4 Tm1 N4 158.0(11) . . . 1_565 ? C3 N8 Tm1 O5 137(7) . . . . ? C3 N8 Tm1 O3 34(7) . . . . ? C3 N8 Tm1 O6 -159(7) . . . . ? C3 N8 Tm1 O2 -77(7) . . . . ? C3 N8 Tm1 O1 -2(7) . . . . ? C3 N8 Tm1 O4 74(7) . . . . ? C3 N8 Tm1 N4 -123(7) . . . 1_565 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.529 _refine_diff_density_min -1.635 _refine_diff_density_rms 0.227 _database_code_depnum_ccdc_archive 'CCDC 881384' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl4 #TrackingRef 'shelxl-Yb.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H42 Mo N14 O6 Yb' _chemical_formula_weight 915.72 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' Mo Mo -1.6832 0.6857 '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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.344(3) _cell_length_b 10.960(2) _cell_length_c 21.261(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.00(3) _cell_angle_gamma 90.00 _cell_volume 3807.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1823 _exptl_absorpt_coefficient_mu 2.825 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6303 _exptl_absorpt_correction_T_max 0.7280 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24836 _diffrn_reflns_av_R_equivalents 0.1265 _diffrn_reflns_av_sigmaI/netI 0.1145 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6598 _reflns_number_gt 4653 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6598 _refine_ls_number_parameters 445 _refine_ls_number_restraints 109 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.1627 _refine_ls_wR_factor_gt 0.1434 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2084(10) -0.3283(12) 0.4408(7) 0.066(4) Uani 1 1 d . . . C2 C 0.3630(10) -0.3080(11) 0.3968(7) 0.061(4) Uani 1 1 d . . . C3 C 0.2422(7) -0.4148(10) 0.3326(5) 0.035(3) Uani 1 1 d . . . C4 C 0.3317(8) -0.2321(10) 0.2823(6) 0.046(3) Uani 1 1 d . . . C5 C 0.1681(9) -0.2284(11) 0.2816(7) 0.060(4) Uani 1 1 d . . . C6 C 0.2593(7) -0.0408(11) 0.3278(6) 0.044(3) Uani 1 1 d . . . C7 C 0.1396(9) -0.1457(13) 0.3922(7) 0.062(4) Uani 1 1 d . . . C8 C 0.2956(9) -0.1146(12) 0.4386(6) 0.060(4) Uani 1 1 d . . . C9 C 0.4707(12) 0.1565(15) 0.4825(8) 0.108(7) Uani 1 1 d . . . H9A H 0.4292 0.0963 0.4896 0.162 Uiso 1 1 calc R . . H9B H 0.4786 0.2048 0.5197 0.162 Uiso 1 1 calc R . . H9C H 0.5210 0.1166 0.4723 0.162 Uiso 1 1 calc R . . C10 C 0.5004(11) 0.3305(19) 0.4108(9) 0.121(8) Uani 1 1 d . . . H10A H 0.5252 0.3079 0.3718 0.182 Uiso 1 1 calc R . . H10B H 0.5422 0.3408 0.4426 0.182 Uiso 1 1 calc R . . H10C H 0.4711 0.4057 0.4053 0.182 Uiso 1 1 calc R . . C11 C 0.3769(7) 0.2152(10) 0.3991(6) 0.046(3) Uani 1 1 d . . . H11 H 0.3444 0.1509 0.4125 0.055 Uiso 1 1 calc R . . C12 C 0.5331(9) 0.5698(14) 0.2553(8) 0.084(5) Uani 1 1 d . . . H12A H 0.5174 0.5870 0.2976 0.126 Uiso 1 1 calc R . . H12B H 0.5342 0.6443 0.2316 0.126 Uiso 1 1 calc R . . H12C H 0.5864 0.5332 0.2556 0.126 Uiso 1 1 calc R . . C13 C 0.4873(11) 0.4503(15) 0.1621(8) 0.092(5) Uani 1 1 d . . . H13A H 0.4715 0.3665 0.1567 0.138 Uiso 1 1 calc R . . H13B H 0.5441 0.4594 0.1522 0.138 Uiso 1 1 calc R . . H13C H 0.4547 0.5007 0.1345 0.138 Uiso 1 1 calc R . . C14 C 0.4127(8) 0.4432(10) 0.2560(6) 0.050(3) Uani 1 1 d . . . H14 H 0.4054 0.4692 0.2971 0.060 Uiso 1 1 calc R . . C15 C 0.2148(9) 0.4936(14) 0.1748(7) 0.069(4) Uani 1 1 d . . . H15 H 0.2462 0.5428 0.2016 0.083 Uiso 1 1 calc R . . C16 C 0.2183(12) 0.6644(14) 0.1043(9) 0.104(6) Uani 1 1 d . . . H16A H 0.2422 0.7058 0.1399 0.157 Uiso 1 1 calc R . . H16B H 0.1709 0.7086 0.0897 0.157 Uiso 1 1 calc R . . H16C H 0.2574 0.6598 0.0713 0.157 Uiso 1 1 calc R . . C17 C 0.1509(16) 0.464(2) 0.0785(10) 0.157(11) Uani 1 1 d . . . H17A H 0.1851 0.4483 0.0432 0.235 Uiso 1 1 calc R . . H17B H 0.1019 0.5050 0.0643 0.235 Uiso 1 1 calc R . . H17C H 0.1369 0.3889 0.0984 0.235 Uiso 1 1 calc R . . C18 C 0.1475(14) 0.301(2) 0.4009(11) 0.117(4) Uani 1 1 d U . . H18 H 0.1698 0.3780 0.4089 0.140 Uiso 1 1 calc R . . C19 C 0.0721(17) 0.358(2) 0.4930(13) 0.173(8) Uani 1 1 d U . . H19A H 0.0158 0.3828 0.4908 0.260 Uiso 1 1 calc R . . H19B H 0.1067 0.4281 0.4880 0.260 Uiso 1 1 calc R . . H19C H 0.0835 0.3209 0.5332 0.260 Uiso 1 1 calc R . . C20 C 0.0297(16) 0.180(2) 0.4449(14) 0.192(9) Uani 1 1 d DU . . H20A H -0.0243 0.2136 0.4406 0.288 Uiso 1 1 calc R . . H20B H 0.0341 0.1349 0.4836 0.288 Uiso 1 1 calc R . . H20C H 0.0397 0.1261 0.4102 0.288 Uiso 1 1 calc R . . C21 C 0.0864(11) 0.1191(16) 0.2520(9) 0.091(4) Uani 1 1 d U . . H21 H 0.0952 0.0776 0.2897 0.109 Uiso 1 1 calc R . . C22 C 0.0123(15) 0.092(2) 0.1568(12) 0.152(7) Uani 1 1 d U . . H22A H -0.0445 0.1134 0.1528 0.228 Uiso 1 1 calc R . . H22B H 0.0230 0.0209 0.1319 0.228 Uiso 1 1 calc R . . H22C H 0.0453 0.1586 0.1425 0.228 Uiso 1 1 calc R . . C23 C -0.0219(13) -0.026(2) 0.2446(10) 0.134(7) Uani 1 1 d U . . H23A H -0.0100 -0.1030 0.2252 0.202 Uiso 1 1 calc R . . H23B H -0.0780 -0.0048 0.2363 0.202 Uiso 1 1 calc R . . H23C H -0.0126 -0.0321 0.2892 0.202 Uiso 1 1 calc R . . C24 C 0.3038(9) 0.1693(13) 0.1422(8) 0.069(4) Uani 1 1 d . . . H24 H 0.3202 0.2461 0.1287 0.082 Uiso 1 1 calc R . . C25 C 0.3348(15) 0.101(2) 0.0373(9) 0.148(9) Uani 1 1 d . . . H25A H 0.3162 0.1793 0.0221 0.222 Uiso 1 1 calc R . . H25B H 0.3143 0.0382 0.0100 0.222 Uiso 1 1 calc R . . H25C H 0.3935 0.0997 0.0381 0.222 Uiso 1 1 calc R . . C26 C 0.2820(14) -0.0366(13) 0.1198(9) 0.123(8) Uani 1 1 d . . . H26A H 0.3288 -0.0894 0.1183 0.184 Uiso 1 1 calc R . . H26B H 0.2400 -0.0669 0.0918 0.184 Uiso 1 1 calc R . . H26C H 0.2618 -0.0344 0.1619 0.184 Uiso 1 1 calc R . . Mo1 Mo 0.25033(6) -0.22546(8) 0.36171(4) 0.0376(3) Uani 1 1 d . . . N1 N 0.2393(6) -0.5164(8) 0.3179(4) 0.041(2) Uani 1 1 d . . . N2 N 0.1259(8) -0.2326(10) 0.2381(6) 0.075(4) Uani 1 1 d . . . N3 N 0.1814(10) -0.3821(12) 0.4807(6) 0.098(5) Uani 1 1 d . . . N4 N 0.4218(9) -0.3553(12) 0.4143(6) 0.087(4) Uani 1 1 d . . . N5 N 0.3210(9) -0.0522(11) 0.4792(6) 0.088(4) Uani 1 1 d . . . N6 N 0.3738(8) -0.2347(11) 0.2404(6) 0.076(4) Uani 1 1 d . . . N7 N 0.0803(10) -0.1033(14) 0.4076(7) 0.104(5) Uani 1 1 d . . . N8 N 0.2608(5) 0.0585(9) 0.3132(4) 0.040(2) Uani 1 1 d . . . N9 N 0.0312(8) 0.0678(12) 0.2189(7) 0.084(3) Uani 1 1 d U . . N10 N 0.3046(8) 0.0816(12) 0.1013(6) 0.077(4) Uani 1 1 d . . . N11 N 0.1942(8) 0.5412(11) 0.1228(6) 0.076(4) Uani 1 1 d . . . N12 N 0.4747(6) 0.4867(9) 0.2267(5) 0.052(3) Uani 1 1 d . . . N13 N 0.4448(7) 0.2362(9) 0.4297(6) 0.060(3) Uani 1 1 d . . . N14 N 0.0873(11) 0.2741(16) 0.4452(8) 0.114(4) Uani 1 1 d DU . . O1 O 0.1992(5) 0.3920(8) 0.1949(4) 0.059(2) Uani 1 1 d . . . O2 O 0.2837(6) 0.1596(7) 0.1961(4) 0.060(2) Uani 1 1 d . . . O3 O 0.1269(6) 0.1986(9) 0.2488(5) 0.078(3) Uani 1 1 d U . . O4 O 0.1723(7) 0.2656(9) 0.3655(6) 0.086(3) Uani 1 1 d U . . O5 O 0.3529(5) 0.2751(7) 0.3535(4) 0.049(2) Uani 1 1 d . . . O6 O 0.3618(5) 0.3692(7) 0.2338(4) 0.053(2) Uani 1 1 d . . . Yb1 Yb 0.24917(3) 0.27655(4) 0.27883(2) 0.03527(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.117(13) 0.030(7) 0.050(9) 0.013(6) -0.009(8) 0.002(8) C2 0.088(11) 0.035(8) 0.059(9) -0.003(6) -0.017(8) 0.009(7) C3 0.049(7) 0.030(7) 0.025(6) 0.013(5) 0.008(5) -0.001(5) C4 0.057(8) 0.018(6) 0.061(9) 0.009(6) -0.002(6) 0.009(5) C5 0.075(10) 0.044(8) 0.061(9) -0.008(7) -0.005(7) 0.020(7) C6 0.048(7) 0.030(7) 0.054(8) 0.001(6) -0.001(6) 0.007(6) C7 0.068(10) 0.062(10) 0.059(9) 0.004(7) 0.026(7) 0.001(8) C8 0.095(11) 0.042(8) 0.044(8) 0.011(6) -0.007(7) -0.003(7) C9 0.150(17) 0.075(11) 0.095(13) 0.027(10) -0.081(12) -0.010(11) C10 0.079(13) 0.157(19) 0.125(18) 0.030(14) -0.040(12) -0.056(13) C11 0.050(7) 0.027(6) 0.061(8) 0.001(6) -0.009(6) 0.002(6) C12 0.055(9) 0.078(11) 0.119(15) -0.018(9) 0.002(9) -0.035(8) C13 0.098(13) 0.106(14) 0.073(12) -0.017(10) 0.023(10) -0.018(10) C14 0.065(9) 0.024(7) 0.062(9) 0.004(6) 0.001(7) 0.008(6) C15 0.078(11) 0.062(10) 0.067(11) 0.000(8) 0.000(8) 0.001(8) C16 0.162(19) 0.060(10) 0.091(14) 0.015(10) 0.006(12) 0.001(11) C17 0.20(3) 0.17(2) 0.096(17) 0.042(15) -0.073(17) -0.062(19) C18 0.115(7) 0.122(7) 0.113(7) 0.002(6) 0.025(6) 0.000(6) C19 0.178(11) 0.168(11) 0.175(11) -0.012(9) 0.007(9) 0.004(9) C20 0.192(12) 0.189(11) 0.195(12) -0.004(9) 0.001(9) -0.004(9) C21 0.077(6) 0.084(6) 0.111(6) -0.002(6) -0.013(6) -0.006(5) C22 0.147(10) 0.161(10) 0.147(11) 0.002(8) 0.002(8) 0.009(8) C23 0.126(10) 0.132(10) 0.145(10) 0.014(8) 0.004(8) 0.001(8) C24 0.083(11) 0.036(8) 0.087(12) 0.010(8) 0.008(9) -0.001(7) C25 0.19(3) 0.18(2) 0.076(15) 0.018(15) 0.039(15) 0.019(18) C26 0.22(2) 0.030(9) 0.114(16) 0.003(9) 0.004(15) -0.018(12) Mo1 0.0542(6) 0.0214(5) 0.0371(6) -0.0002(4) -0.0018(4) 0.0002(5) N1 0.060(6) 0.010(5) 0.053(6) 0.001(4) 0.004(5) -0.012(4) N2 0.080(9) 0.065(8) 0.078(9) -0.017(7) -0.034(7) 0.018(6) N3 0.173(15) 0.069(9) 0.051(9) 0.021(7) 0.004(9) -0.006(9) N4 0.100(11) 0.072(9) 0.088(10) -0.009(7) -0.050(8) 0.019(8) N5 0.129(12) 0.075(9) 0.059(9) -0.027(7) -0.010(8) -0.046(8) N6 0.082(9) 0.074(9) 0.072(9) 0.005(7) 0.022(7) 0.012(7) N7 0.098(12) 0.114(12) 0.101(12) 0.020(9) 0.029(9) 0.012(9) N8 0.046(6) 0.033(6) 0.040(6) 0.000(4) -0.001(4) 0.009(4) N9 0.066(6) 0.085(6) 0.101(6) -0.005(5) -0.016(5) -0.008(5) N10 0.095(10) 0.085(10) 0.051(8) -0.021(7) 0.022(7) 0.003(7) N11 0.105(10) 0.067(8) 0.055(8) 0.028(6) -0.012(7) 0.000(7) N12 0.041(6) 0.042(6) 0.073(8) 0.011(5) 0.016(5) 0.000(5) N13 0.063(7) 0.036(6) 0.079(8) 0.000(5) -0.030(6) -0.005(5) N14 0.114(7) 0.121(7) 0.108(7) -0.002(6) 0.033(6) -0.013(6) O1 0.071(6) 0.042(5) 0.063(6) 0.009(4) -0.010(5) -0.008(5) O2 0.095(7) 0.041(5) 0.045(6) 0.000(4) 0.010(5) -0.005(5) O3 0.061(5) 0.060(5) 0.113(6) 0.018(5) -0.011(5) -0.022(4) O4 0.088(6) 0.081(6) 0.091(6) -0.010(5) 0.057(5) 0.014(5) O5 0.056(5) 0.034(4) 0.056(5) 0.011(4) -0.013(4) -0.004(4) O6 0.050(5) 0.046(5) 0.065(6) 0.000(4) 0.012(4) -0.015(4) Yb1 0.0385(3) 0.0226(3) 0.0447(3) 0.0011(2) 0.00011(19) -0.0026(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 C1 N3 1.129(17) . ? C1 Mo1 2.146(14) . ? C2 N4 1.148(16) . ? C2 Mo1 2.172(15) . ? C3 N1 1.157(12) . ? C3 Mo1 2.169(11) . ? C4 N6 1.135(16) . ? C4 Mo1 2.169(14) . ? C5 N2 1.144(17) . ? C5 Mo1 2.152(15) . ? C6 N8 1.132(13) . ? C6 Mo1 2.154(12) . ? C7 N7 1.128(17) . ? C7 Mo1 2.121(15) . ? C8 N5 1.171(16) . ? C8 Mo1 2.158(14) . ? C9 N13 1.478(17) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 N13 1.439(18) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O5 1.230(13) . ? C11 N13 1.295(15) . ? C11 H11 0.9300 . ? C12 N12 1.445(16) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N12 1.449(18) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 O6 1.248(14) . ? C14 N12 1.289(15) . ? C14 H14 0.9300 . ? C15 O1 1.221(15) . ? C15 N11 1.265(17) . ? C15 H15 0.9300 . ? C16 N11 1.462(18) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N11 1.44(2) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 O4 0.95(2) . ? C18 N14 1.41(2) . ? C18 H18 0.9300 . ? C19 N14 1.40(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N14 1.399(10) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 O3 1.097(17) . ? C21 N9 1.266(19) . ? C21 H21 0.9300 . ? C22 N9 1.38(2) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 N9 1.46(2) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 O2 1.203(17) . ? C24 N10 1.296(18) . ? C24 H24 0.9300 . ? C25 N10 1.47(2) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 N10 1.405(18) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? N1 Yb1 2.422(9) 1_545 ? N8 Yb1 2.505(10) . ? O1 Yb1 2.324(8) . ? O2 Yb1 2.256(9) . ? O3 Yb1 2.255(9) . ? O4 Yb1 2.252(10) . ? O5 Yb1 2.302(8) . ? O6 Yb1 2.323(8) . ? Yb1 N1 2.422(9) 1_565 ? 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 N3 C1 Mo1 175.6(15) . . ? N4 C2 Mo1 177.6(12) . . ? N1 C3 Mo1 178.5(10) . . ? N6 C4 Mo1 179.4(12) . . ? N2 C5 Mo1 177.9(12) . . ? N8 C6 Mo1 175.4(11) . . ? N7 C7 Mo1 179.1(15) . . ? N5 C8 Mo1 178.2(12) . . ? N13 C9 H9A 109.5 . . ? N13 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N13 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N13 C10 H10A 109.5 . . ? N13 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N13 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 N13 124.1(12) . . ? O5 C11 H11 118.0 . . ? N13 C11 H11 118.0 . . ? N12 C12 H12A 109.5 . . ? N12 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N12 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N12 C13 H13A 109.5 . . ? N12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O6 C14 N12 125.6(13) . . ? O6 C14 H14 117.2 . . ? N12 C14 H14 117.2 . . ? O1 C15 N11 128.9(15) . . ? O1 C15 H15 115.6 . . ? N11 C15 H15 115.6 . . ? N11 C16 H16A 109.5 . . ? N11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N11 C17 H17A 109.5 . . ? N11 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N11 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 N14 139(3) . . ? O4 C18 H18 110.3 . . ? N14 C18 H18 110.3 . . ? N14 C19 H19A 109.5 . . ? N14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N14 C20 H20A 109.5 . . ? N14 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O3 C21 N9 138(2) . . ? O3 C21 H21 111.0 . . ? N9 C21 H21 111.0 . . ? N9 C22 H22A 109.5 . . ? N9 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N9 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N9 C23 H23A 109.5 . . ? N9 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N9 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O2 C24 N10 125.4(14) . . ? O2 C24 H24 117.3 . . ? N10 C24 H24 117.3 . . ? N10 C25 H25A 109.5 . . ? N10 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N10 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N10 C26 H26A 109.5 . . ? N10 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N10 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C7 Mo1 C1 72.0(5) . . ? C7 Mo1 C5 73.9(5) . . ? C1 Mo1 C5 114.1(6) . . ? C7 Mo1 C6 77.2(5) . . ? C1 Mo1 C6 141.3(5) . . ? C5 Mo1 C6 78.1(5) . . ? C7 Mo1 C8 79.6(6) . . ? C1 Mo1 C8 79.2(5) . . ? C5 Mo1 C8 144.1(5) . . ? C6 Mo1 C8 72.6(4) . . ? C7 Mo1 C4 142.1(5) . . ? C1 Mo1 C4 143.2(5) . . ? C5 Mo1 C4 76.4(5) . . ? C6 Mo1 C4 74.0(4) . . ? C8 Mo1 C4 113.7(5) . . ? C7 Mo1 C3 115.6(5) . . ? C1 Mo1 C3 72.7(4) . . ? C5 Mo1 C3 74.1(4) . . ? C6 Mo1 C3 143.8(4) . . ? C8 Mo1 C3 140.7(4) . . ? C4 Mo1 C3 77.4(4) . . ? C7 Mo1 C2 142.2(6) . . ? C1 Mo1 C2 78.1(6) . . ? C5 Mo1 C2 141.2(5) . . ? C6 Mo1 C2 116.3(5) . . ? C8 Mo1 C2 72.3(5) . . ? C4 Mo1 C2 74.1(5) . . ? C3 Mo1 C2 75.4(4) . . ? C3 N1 Yb1 172.4(8) . 1_545 ? C6 N8 Yb1 174.3(9) . . ? C21 N9 C22 126.4(18) . . ? C21 N9 C23 121.9(17) . . ? C22 N9 C23 111.7(16) . . ? C24 N10 C26 119.4(14) . . ? C24 N10 C25 121.2(15) . . ? C26 N10 C25 119.2(14) . . ? C15 N11 C17 116.9(14) . . ? C15 N11 C16 123.1(15) . . ? C17 N11 C16 119.8(14) . . ? C14 N12 C12 123.2(13) . . ? C14 N12 C13 118.8(12) . . ? C12 N12 C13 117.9(12) . . ? C11 N13 C10 121.8(12) . . ? C11 N13 C9 120.5(12) . . ? C10 N13 C9 117.5(12) . . ? C19 N14 C20 111(2) . . ? C19 N14 C18 118.9(19) . . ? C20 N14 C18 129(2) . . ? C15 O1 Yb1 133.8(9) . . ? C24 O2 Yb1 140.3(9) . . ? C21 O3 Yb1 144.6(12) . . ? C18 O4 Yb1 151.9(18) . . ? C11 O5 Yb1 140.3(8) . . ? C14 O6 Yb1 131.1(8) . . ? O4 Yb1 O3 73.0(4) . . ? O4 Yb1 O2 139.3(4) . . ? O3 Yb1 O2 78.3(4) . . ? O4 Yb1 O5 81.4(4) . . ? O3 Yb1 O5 146.2(3) . . ? O2 Yb1 O5 110.0(3) . . ? O4 Yb1 O6 144.9(4) . . ? O3 Yb1 O6 138.9(4) . . ? O2 Yb1 O6 73.5(3) . . ? O5 Yb1 O6 73.0(3) . . ? O4 Yb1 O1 117.6(4) . . ? O3 Yb1 O1 72.0(3) . . ? O2 Yb1 O1 78.5(3) . . ? O5 Yb1 O1 141.1(3) . . ? O6 Yb1 O1 73.5(3) . . ? O4 Yb1 N1 74.2(3) . 1_565 ? O3 Yb1 N1 112.8(3) . 1_565 ? O2 Yb1 N1 144.9(3) . 1_565 ? O5 Yb1 N1 79.8(3) . 1_565 ? O6 Yb1 N1 77.8(3) . 1_565 ? O1 Yb1 N1 74.3(3) . 1_565 ? O4 Yb1 N8 75.6(3) . . ? O3 Yb1 N8 77.5(3) . . ? O2 Yb1 N8 70.5(3) . . ? O5 Yb1 N8 75.0(3) . . ? O6 Yb1 N8 118.7(3) . . ? O1 Yb1 N8 140.1(3) . . ? N1 Yb1 N8 143.0(3) 1_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 C7 Mo1 C1 -131(92) . . . . ? N7 C7 Mo1 C5 -9(92) . . . . ? N7 C7 Mo1 C6 72(92) . . . . ? N7 C7 Mo1 C8 147(92) . . . . ? N7 C7 Mo1 C4 31(92) . . . . ? N7 C7 Mo1 C3 -72(92) . . . . ? N7 C7 Mo1 C2 -171(100) . . . . ? N3 C1 Mo1 C7 45(17) . . . . ? N3 C1 Mo1 C5 -18(17) . . . . ? N3 C1 Mo1 C6 84(17) . . . . ? N3 C1 Mo1 C8 127(17) . . . . ? N3 C1 Mo1 C4 -117(17) . . . . ? N3 C1 Mo1 C3 -80(17) . . . . ? N3 C1 Mo1 C2 -159(17) . . . . ? N2 C5 Mo1 C7 -161(40) . . . . ? N2 C5 Mo1 C1 -100(40) . . . . ? N2 C5 Mo1 C6 119(40) . . . . ? N2 C5 Mo1 C8 155(39) . . . . ? N2 C5 Mo1 C4 43(40) . . . . ? N2 C5 Mo1 C3 -38(40) . . . . ? N2 C5 Mo1 C2 1(40) . . . . ? N8 C6 Mo1 C7 28(13) . . . . ? N8 C6 Mo1 C1 -10(13) . . . . ? N8 C6 Mo1 C5 104(13) . . . . ? N8 C6 Mo1 C8 -55(13) . . . . ? N8 C6 Mo1 C4 -177(100) . . . . ? N8 C6 Mo1 C3 144(13) . . . . ? N8 C6 Mo1 C2 -115(13) . . . . ? N5 C8 Mo1 C7 -103(46) . . . . ? N5 C8 Mo1 C1 -176(100) . . . . ? N5 C8 Mo1 C5 -60(47) . . . . ? N5 C8 Mo1 C6 -23(46) . . . . ? N5 C8 Mo1 C4 40(46) . . . . ? N5 C8 Mo1 C3 139(46) . . . . ? N5 C8 Mo1 C2 103(46) . . . . ? N6 C4 Mo1 C7 9(100) . . . . ? N6 C4 Mo1 C1 161(100) . . . . ? N6 C4 Mo1 C5 48(100) . . . . ? N6 C4 Mo1 C6 -33(100) . . . . ? N6 C4 Mo1 C8 -95(100) . . . . ? N6 C4 Mo1 C3 125(100) . . . . ? N6 C4 Mo1 C2 -157(100) . . . . ? N1 C3 Mo1 C7 -132(37) . . . . ? N1 C3 Mo1 C1 -72(37) . . . . ? N1 C3 Mo1 C5 166(37) . . . . ? N1 C3 Mo1 C6 125(37) . . . . ? N1 C3 Mo1 C8 -26(37) . . . . ? N1 C3 Mo1 C4 86(37) . . . . ? N1 C3 Mo1 C2 10(37) . . . . ? N4 C2 Mo1 C7 118(36) . . . . ? N4 C2 Mo1 C1 80(36) . . . . ? N4 C2 Mo1 C5 -34(36) . . . . ? N4 C2 Mo1 C6 -138(36) . . . . ? N4 C2 Mo1 C8 163(36) . . . . ? N4 C2 Mo1 C4 -75(36) . . . . ? N4 C2 Mo1 C3 5(36) . . . . ? Mo1 C3 N1 Yb1 -73(39) . . . 1_545 ? Mo1 C6 N8 Yb1 -65(19) . . . . ? O3 C21 N9 C22 12(4) . . . . ? O3 C21 N9 C23 -167(2) . . . . ? O2 C24 N10 C26 -1(3) . . . . ? O2 C24 N10 C25 -176.4(17) . . . . ? O1 C15 N11 C17 -5(3) . . . . ? O1 C15 N11 C16 -179.2(15) . . . . ? O6 C14 N12 C12 -178.2(13) . . . . ? O6 C14 N12 C13 1.2(19) . . . . ? O5 C11 N13 C10 -3(2) . . . . ? O5 C11 N13 C9 -177.5(14) . . . . ? O4 C18 N14 C19 178(3) . . . . ? O4 C18 N14 C20 -12(5) . . . . ? N11 C15 O1 Yb1 166.9(12) . . . . ? N10 C24 O2 Yb1 -165.3(11) . . . . ? N9 C21 O3 Yb1 -151.0(18) . . . . ? N14 C18 O4 Yb1 165.5(19) . . . . ? N13 C11 O5 Yb1 174.6(9) . . . . ? N12 C14 O6 Yb1 178.2(8) . . . . ? C18 O4 Yb1 O3 -124(4) . . . . ? C18 O4 Yb1 O2 -171(4) . . . . ? C18 O4 Yb1 O5 78(4) . . . . ? C18 O4 Yb1 O6 35(4) . . . . ? C18 O4 Yb1 O1 -66(4) . . . . ? C18 O4 Yb1 N1 -3(4) . . . 1_565 ? C18 O4 Yb1 N8 155(4) . . . . ? C21 O3 Yb1 O4 -69(2) . . . . ? C21 O3 Yb1 O2 82(2) . . . . ? C21 O3 Yb1 O5 -26(3) . . . . ? C21 O3 Yb1 O6 129(2) . . . . ? C21 O3 Yb1 O1 164(2) . . . . ? C21 O3 Yb1 N1 -133(2) . . . 1_565 ? C21 O3 Yb1 N8 10(2) . . . . ? C24 O2 Yb1 O4 151.8(15) . . . . ? C24 O2 Yb1 O3 106.2(16) . . . . ? C24 O2 Yb1 O5 -107.9(16) . . . . ? C24 O2 Yb1 O6 -43.5(16) . . . . ? C24 O2 Yb1 O1 32.5(16) . . . . ? C24 O2 Yb1 N1 -7.0(19) . . . 1_565 ? C24 O2 Yb1 N8 -173.0(17) . . . . ? C11 O5 Yb1 O4 52.6(13) . . . . ? C11 O5 Yb1 O3 12.0(16) . . . . ? C11 O5 Yb1 O2 -86.9(13) . . . . ? C11 O5 Yb1 O6 -151.7(13) . . . . ? C11 O5 Yb1 O1 176.6(11) . . . . ? C11 O5 Yb1 N1 128.0(13) . . . 1_565 ? C11 O5 Yb1 N8 -24.6(12) . . . . ? C14 O6 Yb1 O4 3.7(13) . . . . ? C14 O6 Yb1 O3 152.5(9) . . . . ? C14 O6 Yb1 O2 -158.9(11) . . . . ? C14 O6 Yb1 O5 -41.3(10) . . . . ? C14 O6 Yb1 O1 118.5(10) . . . . ? C14 O6 Yb1 N1 41.6(10) . . . 1_565 ? C14 O6 Yb1 N8 -102.9(10) . . . . ? C15 O1 Yb1 O4 102.3(13) . . . . ? C15 O1 Yb1 O3 161.1(14) . . . . ? C15 O1 Yb1 O2 -117.6(13) . . . . ? C15 O1 Yb1 O5 -10.0(15) . . . . ? C15 O1 Yb1 O6 -41.6(13) . . . . ? C15 O1 Yb1 N1 40.1(13) . . . 1_565 ? C15 O1 Yb1 N8 -156.9(12) . . . . ? C6 N8 Yb1 O4 64(9) . . . . ? C6 N8 Yb1 O3 -12(9) . . . . ? C6 N8 Yb1 O2 -93(9) . . . . ? C6 N8 Yb1 O5 149(9) . . . . ? C6 N8 Yb1 O6 -151(9) . . . . ? C6 N8 Yb1 O1 -52(9) . . . . ? C6 N8 Yb1 N1 100(9) . . . 1_565 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.425 _refine_diff_density_min -1.243 _refine_diff_density_rms 0.160 _database_code_depnum_ccdc_archive 'CCDC 881385'