# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # 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_ss150b _audit_creation_method SHELXL-97 _chemical_name_systematic ; (4,4'-Di-tert-butylbiphenyl-2,2'-bis((2-oxy- 3,5-di-tert-butylphenyl)amido)-(3,5-di-tert-butylphenylcatecholato)- molybdenum(VI) sesquibenzene solvate ; _chemical_name_common '(tBuClip)Mo(3,5-tBu2Cat) . 1.5 C6H6' _chemical_melting_point ? _chemical_formula_moiety 'C62 H84 Mo N2 O4, 1.5 (C6 H6)' _chemical_formula_sum 'C71 H93 Mo N2 O4' _chemical_formula_weight 1134.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 '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 9.6883(2) _cell_length_b 24.4093(5) _cell_length_c 27.7995(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.0270(10) _cell_angle_gamma 90.00 _cell_volume 6473.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9972 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 69.21 _exptl_crystal_description rod _exptl_crystal_colour purple _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid 0.76 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2428 _exptl_absorpt_coefficient_mu 2.015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3025 _exptl_absorpt_correction_T_max 0.8088 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. Madison, WI USA. ; _exptl_crystal_recrystallization_method ; Crystals were grown from benzene layered with acetonitrile ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 53342 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 69.56 _reflns_number_total 11671 _reflns_number_gt 10611 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. The crystal was found to be twinned by examination in the TwinRotMat function within the program PLATON. The twin law was found to be [ -1 0 0 0 -1 0 1 0 1 ], which was applied with a BASF refined to 0.064. Inclusion of this twin law drastically improved the model and eliminated all of the inconsistent equvialents. ; _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^)+(0.0530P)^2^+4.5950P] 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 11671 _refine_ls_number_parameters 724 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1000 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Mo Mo 0.48614(2) 0.436686(8) 0.772496(7) 0.01375(6) Uani 1 1 d . . . O1 O 0.40650(19) 0.39716(7) 0.82422(6) 0.0151(4) Uani 1 1 d . . . N1 N 0.6317(2) 0.38429(8) 0.80072(7) 0.0155(4) Uani 1 1 d . . . N2 N 0.6095(2) 0.49667(8) 0.80291(7) 0.0146(4) Uani 1 1 d . . . O2 O 0.33979(19) 0.49223(7) 0.77926(6) 0.0178(4) Uani 1 1 d . . . O3 O 0.3807(2) 0.38509(7) 0.72178(6) 0.0211(4) Uani 1 1 d . . . O4 O 0.53005(19) 0.46488(7) 0.71130(6) 0.0153(4) Uani 1 1 d . . . C11 C 0.6162(3) 0.35107(10) 0.83911(9) 0.0149(5) Uani 1 1 d . . . C12 C 0.4820(3) 0.35895(9) 0.85076(8) 0.0135(5) Uani 1 1 d . . . C13 C 0.4358(3) 0.32583(10) 0.88672(8) 0.0153(5) Uani 1 1 d . . . C14 C 0.5318(3) 0.28710(10) 0.90893(9) 0.0167(5) Uani 1 1 d . . . H14A H 0.5038 0.2642 0.9331 0.020 Uiso 1 1 calc R . . C15 C 0.6679(3) 0.27942(10) 0.89810(9) 0.0174(5) Uani 1 1 d . . . C16 C 0.7106(3) 0.31213(10) 0.86285(9) 0.0161(5) Uani 1 1 d . . . H16A H 0.8016 0.3083 0.8549 0.019 Uiso 1 1 calc R . . C17 C 0.2904(3) 0.33416(10) 0.89942(9) 0.0167(5) Uani 1 1 d . . . C18 C 0.7612(3) 0.23429(11) 0.92511(10) 0.0205(6) Uani 1 1 d . . . C21 C 0.8537(3) 0.42326(10) 0.78730(9) 0.0169(5) Uani 1 1 d . . . C22 C 0.7484(3) 0.38362(10) 0.77560(9) 0.0163(5) Uani 1 1 d . . . C23 C 0.7484(3) 0.34625(10) 0.73779(9) 0.0195(5) Uani 1 1 d . . . H23A H 0.6744 0.3203 0.7308 0.023 Uiso 1 1 calc R . . C24 C 0.8548(3) 0.34623(11) 0.71003(10) 0.0207(6) Uani 1 1 d . A . C25 C 0.9637(3) 0.38420(11) 0.72291(10) 0.0220(6) Uani 1 1 d . . . H25A H 1.0399 0.3843 0.7055 0.026 Uiso 1 1 calc R . . C26 C 0.9627(3) 0.42151(11) 0.76035(9) 0.0199(6) Uani 1 1 d . . . H26A H 1.0383 0.4466 0.7680 0.024 Uiso 1 1 calc R . . C27 C 0.8504(3) 0.30656(13) 0.66674(11) 0.0294(7) Uani 1 1 d . . . C31 C 0.8558(3) 0.46440(10) 0.82680(9) 0.0164(5) Uani 1 1 d . . . C32 C 0.7431(3) 0.49857(10) 0.83337(9) 0.0155(5) Uani 1 1 d . . . C33 C 0.7633(3) 0.53862(10) 0.87043(9) 0.0173(5) Uani 1 1 d . . . H33A H 0.6858 0.5606 0.8750 0.021 Uiso 1 1 calc R . . C34 C 0.8911(3) 0.54731(11) 0.90039(9) 0.0185(5) Uani 1 1 d . . . C35 C 1.0021(3) 0.51285(11) 0.89389(9) 0.0202(6) Uani 1 1 d . . . H35A H 1.0912 0.5172 0.9141 0.024 Uiso 1 1 calc R . . C36 C 0.9834(3) 0.47260(11) 0.85847(9) 0.0194(5) Uani 1 1 d . . . H36A H 1.0602 0.4495 0.8554 0.023 Uiso 1 1 calc R . . C37 C 0.9145(3) 0.59571(11) 0.93625(9) 0.0220(6) Uani 1 1 d . . . C41 C 0.5438(3) 0.54618(10) 0.78557(8) 0.0160(5) Uani 1 1 d . . . C42 C 0.3970(3) 0.54179(10) 0.77141(9) 0.0167(5) Uani 1 1 d . . . C43 C 0.3176(3) 0.58646(11) 0.75002(9) 0.0213(6) Uani 1 1 d . . . C44 C 0.3922(3) 0.63463(11) 0.74560(9) 0.0221(6) Uani 1 1 d . . . H44A H 0.3410 0.6658 0.7319 0.027 Uiso 1 1 calc R . . C45 C 0.5380(3) 0.64017(10) 0.75998(9) 0.0190(5) Uani 1 1 d . B . C46 C 0.6133(3) 0.59524(10) 0.77948(9) 0.0172(5) Uani 1 1 d . . . H46A H 0.7122 0.5975 0.7888 0.021 Uiso 1 1 calc R . . C47 C 0.1600(3) 0.58116(13) 0.73197(11) 0.0295(7) Uani 1 1 d . . . C48 C 0.6126(3) 0.69506(11) 0.75497(10) 0.0249(6) Uani 1 1 d . . . C51 C 0.3921(3) 0.39513(10) 0.67515(9) 0.0199(6) Uani 1 1 d . . . C52 C 0.4731(3) 0.44082(10) 0.66882(8) 0.0157(5) Uani 1 1 d . . . C53 C 0.4930(3) 0.45841(11) 0.62223(9) 0.0185(5) Uani 1 1 d . . . C54 C 0.4325(3) 0.42558(11) 0.58336(9) 0.0232(6) Uani 1 1 d . . . H54A H 0.4422 0.4363 0.5513 0.028 Uiso 1 1 calc R . . C55 C 0.3579(3) 0.37735(11) 0.58903(10) 0.0249(6) Uani 1 1 d . . . C56 C 0.3353(3) 0.36267(11) 0.63537(10) 0.0258(6) Uani 1 1 d . . . H56A H 0.2820 0.3310 0.6398 0.031 Uiso 1 1 calc R . . C57 C 0.5762(3) 0.51070(11) 0.61680(9) 0.0213(6) Uani 1 1 d . . . C58 C 0.3052(4) 0.34164(13) 0.54368(11) 0.0352(8) Uani 1 1 d . . . C61 C 0.3892(3) 0.55547(14) 0.89982(12) 0.0333(7) Uani 1 1 d . . . H61A H 0.3834 0.5283 0.8751 0.040 Uiso 1 1 calc R . . C62 C 0.4014(4) 0.61009(14) 0.88804(12) 0.0355(7) Uani 1 1 d . . . H62A H 0.4048 0.6206 0.8554 0.043 Uiso 1 1 calc R . . C63 C 0.4085(4) 0.64941(14) 0.92453(14) 0.0421(8) Uani 1 1 d . . . H63A H 0.4172 0.6871 0.9169 0.051 Uiso 1 1 calc R . . C64 C 0.4031(4) 0.63360(16) 0.97204(14) 0.0458(10) Uani 1 1 d . . . H64A H 0.4071 0.6606 0.9968 0.055 Uiso 1 1 calc R . . C65 C 0.3919(4) 0.57931(16) 0.98363(12) 0.0415(8) Uani 1 1 d . . . H65A H 0.3885 0.5688 1.0163 0.050 Uiso 1 1 calc R . . C66 C 0.3855(4) 0.54017(14) 0.94751(12) 0.0357(7) Uani 1 1 d . . . H66A H 0.3786 0.5025 0.9554 0.043 Uiso 1 1 calc R . . C71 C 0.1044(7) 0.5216(3) 0.5383(3) 0.097(2) Uani 1 1 d . . . H71A H 0.1722 0.5373 0.5633 0.117 Uiso 1 1 calc R . . C72 C 0.0054(11) 0.4874(4) 0.5521(4) 0.158(4) Uani 1 1 d . . . H72A H 0.0060 0.4773 0.5851 0.189 Uiso 1 1 calc R . . C73 C -0.1113(9) 0.4658(3) 0.5079(5) 0.148(4) Uani 1 1 d . . . H73A H -0.1863 0.4438 0.5148 0.177 Uiso 1 1 calc R . . C171 C 0.1768(3) 0.32505(12) 0.85438(9) 0.0224(6) Uani 1 1 d . . . H17A H 0.1839 0.2876 0.8422 0.034 Uiso 1 1 calc R . . H17B H 0.1898 0.3513 0.8288 0.034 Uiso 1 1 calc R . . H17C H 0.0842 0.3304 0.8633 0.034 Uiso 1 1 calc R . . C172 C 0.2805(3) 0.39290(11) 0.91913(9) 0.0197(5) Uani 1 1 d . . . H17D H 0.3535 0.3982 0.9479 0.029 Uiso 1 1 calc R . . H17E H 0.1881 0.3984 0.9282 0.029 Uiso 1 1 calc R . . H17F H 0.2937 0.4194 0.8938 0.029 Uiso 1 1 calc R . . C173 C 0.2630(3) 0.29453(11) 0.93967(9) 0.0216(6) Uani 1 1 d . . . H17G H 0.2682 0.2567 0.9283 0.032 Uiso 1 1 calc R . . H17H H 0.1696 0.3015 0.9474 0.032 Uiso 1 1 calc R . . H17I H 0.3339 0.3002 0.9690 0.032 Uiso 1 1 calc R . . C181 C 0.9040(3) 0.23175(12) 0.90868(12) 0.0304(7) Uani 1 1 d . . . H18A H 0.9522 0.2670 0.9153 0.046 Uiso 1 1 calc R . . H18B H 0.8904 0.2240 0.8736 0.046 Uiso 1 1 calc R . . H18C H 0.9607 0.2026 0.9266 0.046 Uiso 1 1 calc R . . C182 C 0.6893(3) 0.17826(11) 0.91411(11) 0.0279(6) Uani 1 1 d . . . H18D H 0.5976 0.1787 0.9244 0.042 Uiso 1 1 calc R . . H18E H 0.7477 0.1495 0.9320 0.042 Uiso 1 1 calc R . . H18F H 0.6769 0.1709 0.8790 0.042 Uiso 1 1 calc R . . C183 C 0.7855(4) 0.24464(13) 0.98041(10) 0.0343(7) Uani 1 1 d . . . H18G H 0.8311 0.2803 0.9875 0.051 Uiso 1 1 calc R . . H18H H 0.8455 0.2157 0.9972 0.051 Uiso 1 1 calc R . . H18I H 0.6953 0.2446 0.9918 0.051 Uiso 1 1 calc R . . C271 C 0.9728(7) 0.3089(3) 0.6412(2) 0.0413(12) Uani 0.560(3) 1 d P A 1 H27A H 1.0453 0.2835 0.6569 0.062 Uiso 0.560(3) 1 calc PR A 1 H27B H 1.0105 0.3462 0.6430 0.062 Uiso 0.560(3) 1 calc PR A 1 H27C H 0.9434 0.2985 0.6069 0.062 Uiso 0.560(3) 1 calc PR A 1 C272 C 0.7127(7) 0.3139(2) 0.6304(2) 0.0384(11) Uani 0.560(3) 1 d P A 1 H27D H 0.6362 0.2960 0.6434 0.058 Uiso 0.560(3) 1 calc PR A 1 H27E H 0.7219 0.2972 0.5991 0.058 Uiso 0.560(3) 1 calc PR A 1 H27F H 0.6922 0.3530 0.6257 0.058 Uiso 0.560(3) 1 calc PR A 1 C273 C 0.8441(8) 0.2445(2) 0.6871(2) 0.0402(12) Uani 0.560(3) 1 d P A 1 H27G H 0.8453 0.2455 0.7224 0.060 Uiso 0.560(3) 1 calc PR A 1 H27H H 0.9254 0.2239 0.6804 0.060 Uiso 0.560(3) 1 calc PR A 1 H27I H 0.7578 0.2268 0.6708 0.060 Uiso 0.560(3) 1 calc PR A 1 C274 C 0.7254(9) 0.2729(3) 0.6579(3) 0.0413(12) Uani 0.440(3) 1 d P A 2 H27J H 0.7239 0.2488 0.6860 0.062 Uiso 0.440(3) 1 calc PR A 2 H27K H 0.7255 0.2506 0.6286 0.062 Uiso 0.440(3) 1 calc PR A 2 H27L H 0.6422 0.2965 0.6532 0.062 Uiso 0.440(3) 1 calc PR A 2 C275 C 0.9874(9) 0.2755(3) 0.6747(3) 0.0384(11) Uani 0.440(3) 1 d P A 2 H27M H 0.9905 0.2505 0.7024 0.058 Uiso 0.440(3) 1 calc PR A 2 H27N H 1.0655 0.3015 0.6815 0.058 Uiso 0.440(3) 1 calc PR A 2 H27O H 0.9949 0.2544 0.6453 0.058 Uiso 0.440(3) 1 calc PR A 2 C276 C 0.8525(10) 0.3470(3) 0.6203(3) 0.0402(12) Uani 0.440(3) 1 d P A 2 H27P H 0.8577 0.3851 0.6314 0.060 Uiso 0.440(3) 1 calc PR A 2 H27Q H 0.7668 0.3416 0.5962 0.060 Uiso 0.440(3) 1 calc PR A 2 H27R H 0.9343 0.3385 0.6052 0.060 Uiso 0.440(3) 1 calc PR A 2 C371 C 1.0096(4) 0.63703(13) 0.91604(11) 0.0316(7) Uani 1 1 d . . . H37A H 0.9636 0.6495 0.8837 0.047 Uiso 1 1 calc R . . H37B H 1.0989 0.6194 0.9134 0.047 Uiso 1 1 calc R . . H37C H 1.0269 0.6685 0.9381 0.047 Uiso 1 1 calc R . . C372 C 0.9880(4) 0.57635(13) 0.98720(10) 0.0313(7) Uani 1 1 d . . . H37D H 0.9279 0.5500 1.0003 0.047 Uiso 1 1 calc R . . H37E H 1.0054 0.6079 1.0092 0.047 Uiso 1 1 calc R . . H37F H 1.0773 0.5589 0.9844 0.047 Uiso 1 1 calc R . . C373 C 0.7776(3) 0.62390(12) 0.94195(10) 0.0277(6) Uani 1 1 d . . . H37G H 0.7296 0.6367 0.9100 0.042 Uiso 1 1 calc R . . H37H H 0.7980 0.6552 0.9641 0.042 Uiso 1 1 calc R . . H37I H 0.7174 0.5979 0.9555 0.042 Uiso 1 1 calc R . . C471 C 0.0969(4) 0.63334(16) 0.70602(16) 0.0489(10) Uani 1 1 d . . . H47A H 0.1419 0.6408 0.6778 0.073 Uiso 1 1 calc R . . H47B H 0.1124 0.6643 0.7287 0.073 Uiso 1 1 calc R . . H47C H -0.0040 0.6282 0.6950 0.073 Uiso 1 1 calc R . . C472 C 0.1313(3) 0.53420(15) 0.69460(11) 0.0357(8) Uani 1 1 d . . . H47D H 0.1700 0.5000 0.7098 0.054 Uiso 1 1 calc R . . H47E H 0.1758 0.5425 0.6664 0.054 Uiso 1 1 calc R . . H47F H 0.0300 0.5302 0.6839 0.054 Uiso 1 1 calc R . . C473 C 0.0864(3) 0.57035(13) 0.77583(12) 0.0328(7) Uani 1 1 d . . . H47G H 0.1248 0.5370 0.7928 0.049 Uiso 1 1 calc R . . H47H H -0.0144 0.5656 0.7643 0.049 Uiso 1 1 calc R . . H47I H 0.1019 0.6015 0.7984 0.049 Uiso 1 1 calc R . . C481 C 0.5196(5) 0.73694(18) 0.7247(2) 0.0493(13) Uani 0.780(5) 1 d P B 1 H48A H 0.4352 0.7429 0.7390 0.074 Uiso 0.780(5) 1 calc PR B 1 H48B H 0.4929 0.7234 0.6912 0.074 Uiso 0.780(5) 1 calc PR B 1 H48C H 0.5707 0.7716 0.7245 0.074 Uiso 0.780(5) 1 calc PR B 1 C482 C 0.7423(5) 0.68581(18) 0.7335(2) 0.0521(14) Uani 0.780(5) 1 d P B 1 H48D H 0.8023 0.6589 0.7533 0.078 Uiso 0.780(5) 1 calc PR B 1 H48E H 0.7932 0.7204 0.7331 0.078 Uiso 0.780(5) 1 calc PR B 1 H48F H 0.7161 0.6720 0.7001 0.078 Uiso 0.780(5) 1 calc PR B 1 C483 C 0.6506(9) 0.7189(2) 0.80673(18) 0.069(2) Uani 0.780(5) 1 d P B 1 H48G H 0.5648 0.7249 0.8202 0.104 Uiso 0.780(5) 1 calc PR B 1 H48H H 0.6996 0.7539 0.8054 0.104 Uiso 0.780(5) 1 calc PR B 1 H48I H 0.7116 0.6932 0.8276 0.104 Uiso 0.780(5) 1 calc PR B 1 C484 C 0.7721(19) 0.6933(7) 0.7715(8) 0.0493(13) Uani 0.220(5) 1 d P B 2 H48J H 0.8133 0.6679 0.7506 0.074 Uiso 0.220(5) 1 calc PR B 2 H48K H 0.7938 0.6808 0.8055 0.074 Uiso 0.220(5) 1 calc PR B 2 H48L H 0.8111 0.7300 0.7689 0.074 Uiso 0.220(5) 1 calc PR B 2 C485 C 0.568(2) 0.7357(7) 0.7869(9) 0.0521(14) Uani 0.220(5) 1 d P B 2 H48M H 0.6159 0.7704 0.7834 0.078 Uiso 0.220(5) 1 calc PR B 2 H48N H 0.5910 0.7231 0.8209 0.078 Uiso 0.220(5) 1 calc PR B 2 H48O H 0.4663 0.7410 0.7781 0.078 Uiso 0.220(5) 1 calc PR B 2 C486 C 0.580(3) 0.7138(8) 0.7011(6) 0.069(2) Uani 0.220(5) 1 d P B 2 H48P H 0.6089 0.6853 0.6801 0.104 Uiso 0.220(5) 1 calc PR B 2 H48Q H 0.6311 0.7478 0.6972 0.104 Uiso 0.220(5) 1 calc PR B 2 H48R H 0.4790 0.7204 0.6917 0.104 Uiso 0.220(5) 1 calc PR B 2 C571 C 0.5778(4) 0.52382(13) 0.56278(10) 0.0356(8) Uani 1 1 d . . . H57A H 0.6208 0.4933 0.5478 0.053 Uiso 1 1 calc R . . H57B H 0.6322 0.5573 0.5605 0.053 Uiso 1 1 calc R . . H57C H 0.4816 0.5292 0.5456 0.053 Uiso 1 1 calc R . . C572 C 0.7277(3) 0.50420(14) 0.64327(11) 0.0327(7) Uani 1 1 d . . . H57D H 0.7710 0.4730 0.6295 0.049 Uiso 1 1 calc R . . H57E H 0.7285 0.4979 0.6781 0.049 Uiso 1 1 calc R . . H57F H 0.7804 0.5376 0.6391 0.049 Uiso 1 1 calc R . . C573 C 0.5079(3) 0.55969(11) 0.63834(10) 0.0263(6) Uani 1 1 d . . . H57G H 0.5049 0.5527 0.6729 0.039 Uiso 1 1 calc R . . H57H H 0.4123 0.5648 0.6204 0.039 Uiso 1 1 calc R . . H57I H 0.5630 0.5928 0.6355 0.039 Uiso 1 1 calc R . . C581 C 0.2394(5) 0.28805(14) 0.55689(12) 0.0526(12) Uani 1 1 d . . . H58A H 0.1586 0.2962 0.5725 0.079 Uiso 1 1 calc R . . H58B H 0.3088 0.2671 0.5794 0.079 Uiso 1 1 calc R . . H58C H 0.2087 0.2666 0.5272 0.079 Uiso 1 1 calc R . . C582 C 0.4307(5) 0.32835(16) 0.51868(13) 0.0517(11) Uani 1 1 d . . . H58D H 0.3992 0.3058 0.4897 0.078 Uiso 1 1 calc R . . H58E H 0.5015 0.3083 0.5415 0.078 Uiso 1 1 calc R . . H58F H 0.4713 0.3625 0.5089 0.078 Uiso 1 1 calc R . . C583 C 0.1953(4) 0.37321(15) 0.50826(11) 0.0469(10) Uani 1 1 d . . . H58G H 0.1150 0.3815 0.5241 0.070 Uiso 1 1 calc R . . H58H H 0.1643 0.3509 0.4790 0.070 Uiso 1 1 calc R . . H58I H 0.2362 0.4075 0.4989 0.070 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.01702(12) 0.01326(10) 0.01142(9) 0.00140(7) 0.00372(8) -0.00017(8) O1 0.0182(10) 0.0152(8) 0.0120(7) 0.0030(6) 0.0033(7) -0.0006(7) N1 0.0160(12) 0.0127(10) 0.0184(10) -0.0005(8) 0.0046(9) 0.0006(8) N2 0.0159(12) 0.0146(10) 0.0134(9) 0.0013(8) 0.0031(9) 0.0013(8) O2 0.0183(10) 0.0164(9) 0.0191(8) 0.0010(7) 0.0046(8) 0.0012(7) O3 0.0317(12) 0.0165(9) 0.0155(8) -0.0010(7) 0.0056(8) -0.0067(8) O4 0.0172(10) 0.0166(9) 0.0122(8) 0.0011(6) 0.0032(7) -0.0003(7) C11 0.0192(15) 0.0109(11) 0.0150(11) -0.0015(9) 0.0038(11) -0.0034(9) C12 0.0161(14) 0.0123(11) 0.0114(10) 0.0000(9) 0.0009(10) -0.0018(9) C13 0.0172(15) 0.0153(12) 0.0132(11) -0.0021(9) 0.0018(11) -0.0034(9) C14 0.0203(15) 0.0154(12) 0.0146(11) 0.0007(9) 0.0032(11) -0.0021(10) C15 0.0196(15) 0.0138(12) 0.0170(11) -0.0029(9) -0.0017(11) -0.0012(10) C16 0.0124(14) 0.0165(12) 0.0192(11) -0.0016(9) 0.0020(11) -0.0013(9) C17 0.0177(15) 0.0176(12) 0.0149(11) 0.0035(9) 0.0032(11) -0.0018(10) C18 0.0199(16) 0.0183(13) 0.0220(13) 0.0019(10) 0.0000(12) 0.0021(10) C21 0.0184(15) 0.0152(12) 0.0173(11) 0.0050(9) 0.0035(11) 0.0029(9) C22 0.0132(14) 0.0180(12) 0.0192(11) 0.0046(10) 0.0071(11) 0.0051(9) C23 0.0193(15) 0.0156(12) 0.0242(13) -0.0003(10) 0.0054(12) 0.0006(10) C24 0.0200(15) 0.0211(13) 0.0216(12) -0.0014(10) 0.0052(12) 0.0034(10) C25 0.0187(15) 0.0249(14) 0.0247(13) 0.0030(11) 0.0106(13) 0.0022(10) C26 0.0173(15) 0.0207(13) 0.0226(13) 0.0037(10) 0.0059(12) -0.0005(10) C27 0.0282(18) 0.0349(17) 0.0267(14) -0.0107(12) 0.0090(14) 0.0050(13) C31 0.0199(15) 0.0160(12) 0.0138(11) 0.0055(9) 0.0046(11) 0.0003(10) C32 0.0153(14) 0.0164(12) 0.0144(11) 0.0051(9) 0.0011(11) -0.0032(9) C33 0.0182(15) 0.0183(12) 0.0160(11) 0.0036(9) 0.0042(11) 0.0012(10) C34 0.0212(16) 0.0210(13) 0.0138(11) 0.0033(10) 0.0048(11) -0.0018(10) C35 0.0166(15) 0.0251(14) 0.0175(12) 0.0024(10) -0.0007(11) -0.0009(10) C36 0.0186(15) 0.0206(13) 0.0194(12) 0.0047(10) 0.0048(11) 0.0021(10) C37 0.0243(17) 0.0253(14) 0.0157(12) -0.0017(10) 0.0012(12) -0.0009(11) C41 0.0198(15) 0.0167(12) 0.0109(10) 0.0006(9) 0.0014(10) 0.0032(10) C42 0.0218(15) 0.0148(12) 0.0145(11) -0.0005(9) 0.0059(11) 0.0012(10) C43 0.0210(16) 0.0263(14) 0.0181(12) 0.0046(10) 0.0078(12) 0.0049(11) C44 0.0248(17) 0.0205(13) 0.0227(13) 0.0073(10) 0.0089(12) 0.0088(11) C45 0.0253(16) 0.0185(13) 0.0142(11) 0.0005(9) 0.0061(11) 0.0019(11) C46 0.0196(15) 0.0194(13) 0.0125(11) -0.0009(9) 0.0026(11) 0.0000(10) C47 0.0182(16) 0.0351(16) 0.0362(16) 0.0165(13) 0.0074(14) 0.0045(12) C48 0.0349(19) 0.0162(13) 0.0225(13) 0.0024(10) 0.0021(13) -0.0029(11) C51 0.0297(17) 0.0173(12) 0.0142(11) -0.0001(10) 0.0078(12) 0.0014(11) C52 0.0201(15) 0.0164(12) 0.0110(10) -0.0023(9) 0.0040(10) 0.0031(10) C53 0.0183(15) 0.0201(13) 0.0180(12) 0.0000(10) 0.0056(11) -0.0002(10) C54 0.0311(17) 0.0264(15) 0.0134(11) 0.0010(10) 0.0075(12) -0.0011(12) C55 0.0343(18) 0.0210(14) 0.0199(13) -0.0039(11) 0.0057(13) -0.0026(12) C56 0.0378(19) 0.0185(13) 0.0225(13) -0.0028(11) 0.0092(13) -0.0072(12) C57 0.0240(16) 0.0261(14) 0.0137(12) 0.0010(10) 0.0026(11) -0.0068(11) C58 0.056(2) 0.0294(16) 0.0223(14) -0.0106(12) 0.0117(15) -0.0134(15) C61 0.0257(18) 0.0411(18) 0.0324(15) -0.0130(13) 0.0026(14) -0.0025(13) C62 0.0268(19) 0.0460(19) 0.0345(16) -0.0012(14) 0.0076(15) 0.0008(14) C63 0.026(2) 0.0355(18) 0.062(2) -0.0091(16) -0.0023(18) 0.0046(14) C64 0.024(2) 0.059(2) 0.049(2) -0.0317(18) -0.0085(17) 0.0121(16) C65 0.0253(19) 0.069(3) 0.0276(15) -0.0089(15) -0.0025(15) 0.0063(16) C66 0.0270(19) 0.0409(18) 0.0370(16) -0.0037(14) -0.0003(15) -0.0028(14) C71 0.059(4) 0.141(6) 0.090(4) -0.061(4) 0.007(3) 0.022(4) C72 0.146(8) 0.137(7) 0.222(11) -0.074(7) 0.123(9) -0.018(6) C73 0.102(6) 0.124(6) 0.247(12) -0.027(8) 0.112(8) 0.022(5) C171 0.0176(15) 0.0296(15) 0.0197(12) 0.0032(11) 0.0026(12) -0.0044(11) C172 0.0184(15) 0.0242(14) 0.0169(11) 0.0014(10) 0.0046(11) 0.0016(10) C173 0.0190(15) 0.0263(14) 0.0206(12) 0.0054(11) 0.0061(12) -0.0017(11) C181 0.0220(17) 0.0261(15) 0.0417(17) 0.0076(13) 0.0017(14) 0.0054(12) C182 0.0267(17) 0.0186(14) 0.0380(16) 0.0054(12) 0.0042(14) 0.0008(11) C183 0.037(2) 0.0377(18) 0.0239(14) 0.0017(12) -0.0055(14) 0.0115(14) C271 0.043(3) 0.042(3) 0.044(3) -0.021(2) 0.020(2) -0.005(2) C272 0.047(3) 0.036(3) 0.035(2) -0.014(2) 0.015(2) 0.007(2) C273 0.061(4) 0.027(2) 0.034(2) -0.0121(18) 0.012(2) 0.003(2) C274 0.043(3) 0.042(3) 0.044(3) -0.021(2) 0.020(2) -0.005(2) C275 0.047(3) 0.036(3) 0.035(2) -0.014(2) 0.015(2) 0.007(2) C276 0.061(4) 0.027(2) 0.034(2) -0.0121(18) 0.012(2) 0.003(2) C371 0.0323(19) 0.0324(16) 0.0300(15) -0.0067(12) 0.0051(14) -0.0095(13) C372 0.034(2) 0.0388(17) 0.0186(13) -0.0047(12) -0.0024(13) 0.0040(13) C373 0.0281(18) 0.0298(15) 0.0237(13) -0.0094(11) 0.0001(13) 0.0003(12) C471 0.0175(18) 0.053(2) 0.075(3) 0.038(2) 0.0054(18) 0.0082(15) C472 0.0183(18) 0.060(2) 0.0264(15) 0.0098(14) -0.0017(14) -0.0053(14) C473 0.0256(17) 0.0314(16) 0.0456(18) 0.0094(14) 0.0180(15) 0.0082(12) C481 0.040(3) 0.026(2) 0.080(3) 0.026(2) 0.005(3) -0.0039(18) C482 0.044(3) 0.023(2) 0.097(4) 0.012(2) 0.031(3) -0.0048(18) C483 0.125(6) 0.041(3) 0.038(2) -0.005(2) 0.002(3) -0.040(3) C484 0.040(3) 0.026(2) 0.080(3) 0.026(2) 0.005(3) -0.0039(18) C485 0.044(3) 0.023(2) 0.097(4) 0.012(2) 0.031(3) -0.0048(18) C486 0.125(6) 0.041(3) 0.038(2) -0.005(2) 0.002(3) -0.040(3) C571 0.049(2) 0.0387(18) 0.0199(14) 0.0037(12) 0.0087(14) -0.0200(15) C572 0.0254(18) 0.0440(18) 0.0298(15) 0.0028(13) 0.0082(14) -0.0094(14) C573 0.0351(18) 0.0192(13) 0.0238(13) 0.0034(11) 0.0033(13) -0.0049(12) C581 0.096(3) 0.0359(19) 0.0289(16) -0.0161(14) 0.018(2) -0.031(2) C582 0.078(3) 0.045(2) 0.0365(18) -0.0241(16) 0.022(2) -0.0152(19) C583 0.064(3) 0.048(2) 0.0245(15) -0.0083(14) -0.0027(17) -0.0215(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo O4 1.9497(16) . ? Mo N1 1.963(2) . ? Mo N2 1.984(2) . ? Mo O2 1.9941(18) . ? Mo O1 1.9952(16) . ? Mo O3 2.0288(18) . ? O1 C12 1.327(3) . ? N1 C11 1.369(3) . ? N1 C22 1.429(3) . ? N2 C41 1.411(3) . ? N2 C32 1.419(3) . ? O2 C42 1.364(3) . ? O3 C51 1.343(3) . ? O4 C52 1.348(3) . ? C11 C16 1.402(4) . ? C11 C12 1.407(4) . ? C12 C13 1.418(3) . ? C13 C14 1.393(4) . ? C13 C17 1.524(4) . ? C14 C15 1.416(4) . ? C14 H14A 0.9500 . ? C15 C16 1.382(4) . ? C15 C18 1.535(3) . ? C16 H16A 0.9500 . ? C17 C171 1.532(4) . ? C17 C173 1.537(3) . ? C17 C172 1.544(3) . ? C18 C181 1.532(4) . ? C18 C183 1.535(4) . ? C18 C182 1.541(4) . ? C21 C26 1.398(4) . ? C21 C22 1.402(4) . ? C21 C31 1.486(3) . ? C22 C23 1.392(4) . ? C23 C24 1.391(4) . ? C23 H23A 0.9500 . ? C24 C25 1.403(4) . ? C24 C27 1.540(4) . ? C25 C26 1.384(4) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C274 1.448(8) . ? C27 C271 1.486(6) . ? C27 C275 1.511(8) . ? C27 C272 1.536(7) . ? C27 C273 1.621(6) . ? C27 C276 1.628(8) . ? C31 C36 1.401(4) . ? C31 C32 1.411(4) . ? C32 C33 1.409(3) . ? C33 C34 1.383(4) . ? C33 H33A 0.9500 . ? C34 C35 1.402(4) . ? C34 C37 1.537(4) . ? C35 C36 1.380(4) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C373 1.526(4) . ? C37 C371 1.537(4) . ? C37 C372 1.545(4) . ? C41 C46 1.398(4) . ? C41 C42 1.413(4) . ? C42 C43 1.405(4) . ? C43 C44 1.397(4) . ? C43 C47 1.527(4) . ? C44 C45 1.406(4) . ? C44 H44A 0.9500 . ? C45 C46 1.375(4) . ? C45 C48 1.540(4) . ? C46 H46A 0.9500 . ? C47 C471 1.537(4) . ? C47 C473 1.539(4) . ? C47 C472 1.539(5) . ? C48 C485 1.447(19) . ? C48 C482 1.499(5) . ? C48 C481 1.516(5) . ? C48 C484 1.534(19) . ? C48 C483 1.537(5) . ? C48 C486 1.546(18) . ? C51 C52 1.393(4) . ? C51 C56 1.393(4) . ? C52 C53 1.409(3) . ? C53 C54 1.390(4) . ? C53 C57 1.530(4) . ? C54 C55 1.405(4) . ? C54 H54A 0.9500 . ? C55 C56 1.391(4) . ? C55 C58 1.544(4) . ? C56 H56A 0.9500 . ? C57 C572 1.531(4) . ? C57 C573 1.537(4) . ? C57 C571 1.539(3) . ? C58 C583 1.527(5) . ? C58 C581 1.528(4) . ? C58 C582 1.536(5) . ? C61 C62 1.383(5) . ? C61 C66 1.384(5) . ? C61 H61A 0.9500 . ? C62 C63 1.389(5) . ? C62 H62A 0.9500 . ? C63 C64 1.386(5) . ? C63 H63A 0.9500 . ? C64 C65 1.373(5) . ? C64 H64A 0.9500 . ? C65 C66 1.380(5) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C71 C73 1.334(11) 3_566 ? C71 C72 1.376(10) . ? C71 H71A 0.9500 . ? C72 C73 1.605(13) . ? C72 H72A 0.9500 . ? C73 C71 1.334(11) 3_566 ? C73 H73A 0.9500 . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? C173 H17G 0.9800 . ? C173 H17H 0.9800 . ? C173 H17I 0.9800 . ? C181 H18A 0.9800 . ? C181 H18B 0.9800 . ? C181 H18C 0.9800 . ? C182 H18D 0.9800 . ? C182 H18E 0.9800 . ? C182 H18F 0.9800 . ? C183 H18G 0.9800 . ? C183 H18H 0.9800 . ? C183 H18I 0.9800 . ? C271 H27A 0.9800 . ? C271 H27B 0.9800 . ? C271 H27C 0.9800 . ? C272 H27D 0.9800 . ? C272 H27E 0.9800 . ? C272 H27F 0.9800 . ? C273 H27G 0.9800 . ? C273 H27H 0.9800 . ? C273 H27I 0.9800 . ? C274 H27J 0.9800 . ? C274 H27K 0.9800 . ? C274 H27L 0.9800 . ? C275 H27M 0.9800 . ? C275 H27N 0.9800 . ? C275 H27O 0.9800 . ? C276 H27P 0.9800 . ? C276 H27Q 0.9800 . ? C276 H27R 0.9800 . ? C371 H37A 0.9800 . ? C371 H37B 0.9800 . ? C371 H37C 0.9800 . ? C372 H37D 0.9800 . ? C372 H37E 0.9800 . ? C372 H37F 0.9800 . ? C373 H37G 0.9800 . ? C373 H37H 0.9800 . ? C373 H37I 0.9800 . ? C471 H47A 0.9800 . ? C471 H47B 0.9800 . ? C471 H47C 0.9800 . ? C472 H47D 0.9800 . ? C472 H47E 0.9800 . ? C472 H47F 0.9800 . ? C473 H47G 0.9800 . ? C473 H47H 0.9800 . ? C473 H47I 0.9800 . ? C481 H48A 0.9800 . ? C481 H48B 0.9800 . ? C481 H48C 0.9800 . ? C482 H48D 0.9800 . ? C482 H48E 0.9800 . ? C482 H48F 0.9800 . ? C483 H48G 0.9800 . ? C483 H48H 0.9800 . ? C483 H48I 0.9800 . ? C484 H48J 0.9800 . ? C484 H48K 0.9800 . ? C484 H48L 0.9800 . ? C485 H48M 0.9800 . ? C485 H48N 0.9800 . ? C485 H48O 0.9800 . ? C486 H48P 0.9800 . ? C486 H48Q 0.9800 . ? C486 H48R 0.9800 . ? C571 H57A 0.9800 . ? C571 H57B 0.9800 . ? C571 H57C 0.9800 . ? C572 H57D 0.9800 . ? C572 H57E 0.9800 . ? C572 H57F 0.9800 . ? C573 H57G 0.9800 . ? C573 H57H 0.9800 . ? C573 H57I 0.9800 . ? C581 H58A 0.9800 . ? C581 H58B 0.9800 . ? C581 H58C 0.9800 . ? C582 H58D 0.9800 . ? C582 H58E 0.9800 . ? C582 H58F 0.9800 . ? C583 H58G 0.9800 . ? C583 H58H 0.9800 . ? C583 H58I 0.9800 . ? 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 O4 Mo N1 109.15(8) . . ? O4 Mo N2 84.52(8) . . ? N1 Mo N2 88.45(9) . . ? O4 Mo O2 96.26(7) . . ? N1 Mo O2 151.42(8) . . ? N2 Mo O2 81.00(8) . . ? O4 Mo O1 165.98(7) . . ? N1 Mo O1 74.80(8) . . ? N2 Mo O1 109.25(7) . . ? O2 Mo O1 83.70(7) . . ? O4 Mo O3 76.87(7) . . ? N1 Mo O3 96.49(8) . . ? N2 Mo O3 161.35(8) . . ? O2 Mo O3 101.97(8) . . ? O1 Mo O3 89.40(7) . . ? C12 O1 Mo 119.71(15) . . ? C11 N1 C22 125.3(2) . . ? C11 N1 Mo 121.94(18) . . ? C22 N1 Mo 112.75(15) . . ? C41 N2 C32 119.1(2) . . ? C41 N2 Mo 106.52(16) . . ? C32 N2 Mo 134.25(16) . . ? C42 O2 Mo 105.82(15) . . ? C51 O3 Mo 116.21(16) . . ? C52 O4 Mo 119.51(15) . . ? N1 C11 C16 128.2(2) . . ? N1 C11 C12 109.2(2) . . ? C16 C11 C12 122.5(2) . . ? O1 C12 C11 114.2(2) . . ? O1 C12 C13 125.6(2) . . ? C11 C12 C13 120.2(2) . . ? C14 C13 C12 115.5(2) . . ? C14 C13 C17 124.1(2) . . ? C12 C13 C17 120.4(2) . . ? C13 C14 C15 124.8(2) . . ? C13 C14 H14A 117.6 . . ? C15 C14 H14A 117.6 . . ? C16 C15 C14 118.6(2) . . ? C16 C15 C18 122.5(2) . . ? C14 C15 C18 118.8(2) . . ? C15 C16 C11 118.3(2) . . ? C15 C16 H16A 120.8 . . ? C11 C16 H16A 120.8 . . ? C13 C17 C171 110.6(2) . . ? C13 C17 C173 111.6(2) . . ? C171 C17 C173 108.3(2) . . ? C13 C17 C172 108.9(2) . . ? C171 C17 C172 110.2(2) . . ? C173 C17 C172 107.3(2) . . ? C181 C18 C183 108.4(3) . . ? C181 C18 C15 111.6(2) . . ? C183 C18 C15 110.3(2) . . ? C181 C18 C182 107.8(2) . . ? C183 C18 C182 109.3(2) . . ? C15 C18 C182 109.4(2) . . ? C26 C21 C22 116.2(2) . . ? C26 C21 C31 120.1(2) . . ? C22 C21 C31 123.6(2) . . ? C23 C22 C21 122.2(2) . . ? C23 C22 N1 118.7(2) . . ? C21 C22 N1 119.0(2) . . ? C24 C23 C22 121.1(3) . . ? C24 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? C23 C24 C25 117.1(2) . . ? C23 C24 C27 120.8(3) . . ? C25 C24 C27 122.1(2) . . ? C26 C25 C24 121.5(2) . . ? C26 C25 H25A 119.2 . . ? C24 C25 H25A 119.2 . . ? C25 C26 C21 121.9(3) . . ? C25 C26 H26A 119.1 . . ? C21 C26 H26A 119.1 . . ? C274 C27 C275 115.3(5) . . ? C271 C27 C272 110.8(4) . . ? C274 C27 C24 113.4(3) . . ? C271 C27 C24 115.7(3) . . ? C275 C27 C24 107.3(3) . . ? C272 C27 C24 110.1(3) . . ? C271 C27 C273 106.5(4) . . ? C272 C27 C273 104.9(4) . . ? C24 C27 C273 108.2(3) . . ? C274 C27 C276 109.6(5) . . ? C275 C27 C276 106.7(5) . . ? C24 C27 C276 103.7(3) . . ? C36 C31 C32 116.9(2) . . ? C36 C31 C21 117.3(2) . . ? C32 C31 C21 125.7(2) . . ? C33 C32 C31 119.5(2) . . ? C33 C32 N2 117.1(2) . . ? C31 C32 N2 123.3(2) . . ? C34 C33 C32 122.9(2) . . ? C34 C33 H33A 118.6 . . ? C32 C33 H33A 118.6 . . ? C33 C34 C35 117.2(2) . . ? C33 C34 C37 121.6(2) . . ? C35 C34 C37 121.0(3) . . ? C36 C35 C34 120.7(3) . . ? C36 C35 H35A 119.7 . . ? C34 C35 H35A 119.7 . . ? C35 C36 C31 122.8(3) . . ? C35 C36 H36A 118.6 . . ? C31 C36 H36A 118.6 . . ? C373 C37 C34 112.4(2) . . ? C373 C37 C371 109.2(2) . . ? C34 C37 C371 107.3(2) . . ? C373 C37 C372 108.2(2) . . ? C34 C37 C372 110.6(2) . . ? C371 C37 C372 109.0(3) . . ? C46 C41 N2 125.2(3) . . ? C46 C41 C42 120.9(2) . . ? N2 C41 C42 113.7(2) . . ? O2 C42 C43 123.2(2) . . ? O2 C42 C41 116.1(2) . . ? C43 C42 C41 120.6(2) . . ? C44 C43 C42 115.9(3) . . ? C44 C43 C47 123.1(2) . . ? C42 C43 C47 121.0(3) . . ? C43 C44 C45 124.5(2) . . ? C43 C44 H44A 117.8 . . ? C45 C44 H44A 117.8 . . ? C46 C45 C44 118.2(2) . . ? C46 C45 C48 120.3(3) . . ? C44 C45 C48 121.5(2) . . ? C45 C46 C41 119.8(3) . . ? C45 C46 H46A 120.1 . . ? C41 C46 H46A 120.1 . . ? C43 C47 C471 112.2(3) . . ? C43 C47 C473 109.2(3) . . ? C471 C47 C473 108.2(3) . . ? C43 C47 C472 109.7(2) . . ? C471 C47 C472 106.9(3) . . ? C473 C47 C472 110.7(3) . . ? C482 C48 C481 109.8(3) . . ? C485 C48 C484 103.3(12) . . ? C482 C48 C483 110.5(4) . . ? C481 C48 C483 106.6(4) . . ? C485 C48 C45 110.2(7) . . ? C482 C48 C45 110.1(3) . . ? C481 C48 C45 113.2(3) . . ? C484 C48 C45 114.4(6) . . ? C483 C48 C45 106.5(3) . . ? C485 C48 C486 111.0(13) . . ? C484 C48 C486 108.9(13) . . ? C45 C48 C486 109.0(7) . . ? O3 C51 C52 114.3(2) . . ? O3 C51 C56 125.1(2) . . ? C52 C51 C56 120.6(2) . . ? O4 C52 C51 113.1(2) . . ? O4 C52 C53 124.9(2) . . ? C51 C52 C53 122.0(2) . . ? C54 C53 C52 115.6(2) . . ? C54 C53 C57 124.2(2) . . ? C52 C53 C57 120.2(2) . . ? C53 C54 C55 123.5(2) . . ? C53 C54 H54A 118.3 . . ? C55 C54 H54A 118.3 . . ? C56 C55 C54 119.1(2) . . ? C56 C55 C58 121.9(3) . . ? C54 C55 C58 119.0(2) . . ? C55 C56 C51 119.0(3) . . ? C55 C56 H56A 120.5 . . ? C51 C56 H56A 120.5 . . ? C53 C57 C572 110.1(2) . . ? C53 C57 C573 109.9(2) . . ? C572 C57 C573 109.6(2) . . ? C53 C57 C571 111.4(2) . . ? C572 C57 C571 108.6(2) . . ? C573 C57 C571 107.3(2) . . ? C583 C58 C581 108.3(3) . . ? C583 C58 C582 109.4(3) . . ? C581 C58 C582 108.9(3) . . ? C583 C58 C55 109.6(3) . . ? C581 C58 C55 112.3(2) . . ? C582 C58 C55 108.3(3) . . ? C62 C61 C66 120.3(3) . . ? C62 C61 H61A 119.8 . . ? C66 C61 H61A 119.8 . . ? C61 C62 C63 119.3(3) . . ? C61 C62 H62A 120.4 . . ? C63 C62 H62A 120.4 . . ? C64 C63 C62 119.9(3) . . ? C64 C63 H63A 120.1 . . ? C62 C63 H63A 120.1 . . ? C65 C64 C63 120.7(3) . . ? C65 C64 H64A 119.7 . . ? C63 C64 H64A 119.7 . . ? C64 C65 C66 119.5(3) . . ? C64 C65 H65A 120.2 . . ? C66 C65 H65A 120.2 . . ? C65 C66 C61 120.3(3) . . ? C65 C66 H66A 119.8 . . ? C61 C66 H66A 119.8 . . ? C73 C71 C72 124.2(7) 3_566 . ? C73 C71 H71A 117.9 3_566 . ? C72 C71 H71A 117.9 . . ? C71 C72 C73 114.7(9) . . ? C71 C72 H72A 122.6 . . ? C73 C72 H72A 122.6 . . ? C71 C73 C72 120.9(8) 3_566 . ? C71 C73 H73A 119.5 3_566 . ? C72 C73 H73A 119.5 . . ? C17 C171 H17A 109.5 . . ? C17 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C17 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C17 C172 H17D 109.5 . . ? C17 C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? C17 C172 H17F 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? C17 C173 H17G 109.5 . . ? C17 C173 H17H 109.5 . . ? H17G C173 H17H 109.5 . . ? C17 C173 H17I 109.5 . . ? H17G C173 H17I 109.5 . . ? H17H C173 H17I 109.5 . . ? C18 C181 H18A 109.5 . . ? C18 C181 H18B 109.5 . . ? H18A C181 H18B 109.5 . . ? C18 C181 H18C 109.5 . . ? H18A C181 H18C 109.5 . . ? H18B C181 H18C 109.5 . . ? C18 C182 H18D 109.5 . . ? C18 C182 H18E 109.5 . . ? H18D C182 H18E 109.5 . . ? C18 C182 H18F 109.5 . . ? H18D C182 H18F 109.5 . . ? H18E C182 H18F 109.5 . . ? C18 C183 H18G 109.5 . . ? C18 C183 H18H 109.5 . . ? H18G C183 H18H 109.5 . . ? C18 C183 H18I 109.5 . . ? H18G C183 H18I 109.5 . . ? H18H C183 H18I 109.5 . . ? C27 C271 H27A 109.5 . . ? C27 C271 H27B 109.5 . . ? H27A C271 H27B 109.5 . . ? C27 C271 H27C 109.5 . . ? H27A C271 H27C 109.5 . . ? H27B C271 H27C 109.5 . . ? C27 C272 H27D 109.5 . . ? C27 C272 H27E 109.5 . . ? H27D C272 H27E 109.5 . . ? C27 C272 H27F 109.5 . . ? H27D C272 H27F 109.5 . . ? H27E C272 H27F 109.5 . . ? C27 C273 H27G 109.5 . . ? C27 C273 H27H 109.5 . . ? H27G C273 H27H 109.5 . . ? C27 C273 H27I 109.5 . . ? H27G C273 H27I 109.5 . . ? H27H C273 H27I 109.5 . . ? C27 C274 H27J 109.5 . . ? C27 C274 H27K 109.5 . . ? H27J C274 H27K 109.5 . . ? C27 C274 H27L 109.5 . . ? H27J C274 H27L 109.5 . . ? H27K C274 H27L 109.5 . . ? C27 C275 H27M 109.5 . . ? C27 C275 H27N 109.5 . . ? H27M C275 H27N 109.5 . . ? C27 C275 H27O 109.5 . . ? H27M C275 H27O 109.5 . . ? H27N C275 H27O 109.5 . . ? C27 C276 H27P 109.5 . . ? C27 C276 H27Q 109.5 . . ? H27P C276 H27Q 109.5 . . ? C27 C276 H27R 109.5 . . ? H27P C276 H27R 109.5 . . ? H27Q C276 H27R 109.5 . . ? C37 C371 H37A 109.5 . . ? C37 C371 H37B 109.5 . . ? H37A C371 H37B 109.5 . . ? C37 C371 H37C 109.5 . . ? H37A C371 H37C 109.5 . . ? H37B C371 H37C 109.5 . . ? C37 C372 H37D 109.5 . . ? C37 C372 H37E 109.5 . . ? H37D C372 H37E 109.5 . . ? C37 C372 H37F 109.5 . . ? H37D C372 H37F 109.5 . . ? H37E C372 H37F 109.5 . . ? C37 C373 H37G 109.5 . . ? C37 C373 H37H 109.5 . . ? H37G C373 H37H 109.5 . . ? C37 C373 H37I 109.5 . . ? H37G C373 H37I 109.5 . . ? H37H C373 H37I 109.5 . . ? C47 C471 H47A 109.5 . . ? C47 C471 H47B 109.5 . . ? H47A C471 H47B 109.5 . . ? C47 C471 H47C 109.5 . . ? H47A C471 H47C 109.5 . . ? H47B C471 H47C 109.5 . . ? C47 C472 H47D 109.5 . . ? C47 C472 H47E 109.5 . . ? H47D C472 H47E 109.5 . . ? C47 C472 H47F 109.5 . . ? H47D C472 H47F 109.5 . . ? H47E C472 H47F 109.5 . . ? C47 C473 H47G 109.5 . . ? C47 C473 H47H 109.5 . . ? H47G C473 H47H 109.5 . . ? C47 C473 H47I 109.5 . . ? H47G C473 H47I 109.5 . . ? H47H C473 H47I 109.5 . . ? C48 C481 H48A 109.5 . . ? C48 C481 H48B 109.5 . . ? H48A C481 H48B 109.5 . . ? C48 C481 H48C 109.5 . . ? H48A C481 H48C 109.5 . . ? H48B C481 H48C 109.5 . . ? C48 C482 H48D 109.5 . . ? C48 C482 H48E 109.5 . . ? H48D C482 H48E 109.5 . . ? C48 C482 H48F 109.5 . . ? H48D C482 H48F 109.5 . . ? H48E C482 H48F 109.5 . . ? C48 C483 H48G 109.5 . . ? C48 C483 H48H 109.5 . . ? H48G C483 H48H 109.5 . . ? C48 C483 H48I 109.5 . . ? H48G C483 H48I 109.5 . . ? H48H C483 H48I 109.5 . . ? C48 C484 H48J 109.5 . . ? C48 C484 H48K 109.5 . . ? H48J C484 H48K 109.5 . . ? C48 C484 H48L 109.5 . . ? H48J C484 H48L 109.5 . . ? H48K C484 H48L 109.5 . . ? C48 C485 H48M 109.5 . . ? C48 C485 H48N 109.5 . . ? H48M C485 H48N 109.5 . . ? C48 C485 H48O 109.5 . . ? H48M C485 H48O 109.5 . . ? H48N C485 H48O 109.5 . . ? C48 C486 H48P 109.5 . . ? C48 C486 H48Q 109.5 . . ? H48P C486 H48Q 109.5 . . ? C48 C486 H48R 109.5 . . ? H48P C486 H48R 109.5 . . ? H48Q C486 H48R 109.5 . . ? C57 C571 H57A 109.5 . . ? C57 C571 H57B 109.5 . . ? H57A C571 H57B 109.5 . . ? C57 C571 H57C 109.5 . . ? H57A C571 H57C 109.5 . . ? H57B C571 H57C 109.5 . . ? C57 C572 H57D 109.5 . . ? C57 C572 H57E 109.5 . . ? H57D C572 H57E 109.5 . . ? C57 C572 H57F 109.5 . . ? H57D C572 H57F 109.5 . . ? H57E C572 H57F 109.5 . . ? C57 C573 H57G 109.5 . . ? C57 C573 H57H 109.5 . . ? H57G C573 H57H 109.5 . . ? C57 C573 H57I 109.5 . . ? H57G C573 H57I 109.5 . . ? H57H C573 H57I 109.5 . . ? C58 C581 H58A 109.5 . . ? C58 C581 H58B 109.5 . . ? H58A C581 H58B 109.5 . . ? C58 C581 H58C 109.5 . . ? H58A C581 H58C 109.5 . . ? H58B C581 H58C 109.5 . . ? C58 C582 H58D 109.5 . . ? C58 C582 H58E 109.5 . . ? H58D C582 H58E 109.5 . . ? C58 C582 H58F 109.5 . . ? H58D C582 H58F 109.5 . . ? H58E C582 H58F 109.5 . . ? C58 C583 H58G 109.5 . . ? C58 C583 H58H 109.5 . . ? H58G C583 H58H 109.5 . . ? C58 C583 H58I 109.5 . . ? H58G C583 H58I 109.5 . . ? H58H C583 H58I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 69.56 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.774 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.063 _database_code_depnum_ccdc_archive 'CCDC 976190' ####################################################################### # # 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_ss156_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; (4,4'-Di-tert-butylbiphenyl-2,2'-bis((2-oxy- 3,5-di-tert-butylphenyl)amido)-\m-bis(3,5-di-tert-butylcatecholato)- molybdenum(VI)-(3,5-di-tert-butylcatecholato)(oxo)molybdenum(VI) sesquibenzene solvate ; _chemical_name_common '(tBuClip)Mo2(O)(Cat)3 . 1.5 C6H6' _chemical_melting_point ? _chemical_formula_moiety 'C90 H124 Mo2 N2 O9, 1.5(C6 H6)' _chemical_formula_sum 'C99 H133 Mo2 N2 O9' _chemical_formula_weight 1686.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.429(3) _cell_length_b 14.825(3) _cell_length_c 25.227(5) _cell_angle_alpha 90.224(5) _cell_angle_beta 103.562(5) _cell_angle_gamma 118.130(5) _cell_volume 4584.8(16) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3802 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 20.65 _exptl_crystal_description 'recatangular tablet' _exptl_crystal_colour brown _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1794 _exptl_absorpt_coefficient_mu 0.329 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9416 _exptl_absorpt_correction_T_max 0.9795 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. Madison, WI USA. ; _exptl_crystal_recrystallization_method ; Crystals were grown from benzene layered with acetonitrile ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 53565 _diffrn_reflns_av_R_equivalents 0.0934 _diffrn_reflns_av_sigmaI/netI 0.1279 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.41 _reflns_number_total 18537 _reflns_number_gt 11227 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.0377P)^2^+1.6848P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 18537 _refine_ls_number_parameters 1009 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1146 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 1.43222(3) 0.33332(3) 0.310911(14) 0.01419(10) Uani 1 1 d . . . Mo2 Mo 1.56584(3) 0.27127(3) 0.233691(14) 0.01243(9) Uani 1 1 d . . . O O 1.4057(2) 0.4322(2) 0.31260(11) 0.0201(7) Uani 1 1 d . . . O1 O 1.7046(2) 0.3729(2) 0.28853(10) 0.0146(6) Uani 1 1 d . . . O2 O 1.4355(2) 0.2283(2) 0.16765(10) 0.0152(6) Uani 1 1 d . . . O11 O 1.5112(2) 0.37849(19) 0.25054(10) 0.0136(6) Uani 1 1 d . . . O12 O 1.6265(2) 0.37905(19) 0.18610(10) 0.0150(6) Uani 1 1 d . . . O21 O 1.5288(2) 0.25308(19) 0.31182(10) 0.0135(6) Uani 1 1 d . . . O22 O 1.5424(2) 0.3847(2) 0.38044(10) 0.0151(6) Uani 1 1 d . . . O31 O 1.3136(2) 0.2304(2) 0.25194(11) 0.0187(7) Uani 1 1 d . . . O32 O 1.3383(2) 0.2363(2) 0.35208(10) 0.0178(6) Uani 1 1 d . . . N1 N 1.6768(2) 0.2322(2) 0.22254(12) 0.0126(7) Uani 1 1 d . . . N2 N 1.4710(3) 0.1153(2) 0.22744(12) 0.0132(7) Uani 1 1 d . . . C11 C 1.7849(3) 0.3046(3) 0.24472(16) 0.0154(9) Uani 1 1 d . . . C12 C 1.7968(3) 0.3867(3) 0.27995(15) 0.0131(9) Uani 1 1 d . . . C13 C 1.9003(3) 0.4726(3) 0.30382(16) 0.0169(9) Uani 1 1 d . . . C14 C 1.9884(3) 0.4666(3) 0.29456(16) 0.0200(10) Uani 1 1 d . . . H14A H 2.0593 0.5223 0.3109 0.024 Uiso 1 1 calc R . . C15 C 1.9802(3) 0.3829(3) 0.26230(16) 0.0180(9) Uani 1 1 d . . . C16 C 1.8776(3) 0.3025(3) 0.23715(16) 0.0162(9) Uani 1 1 d . . . H16A H 1.8695 0.2461 0.2149 0.019 Uiso 1 1 calc R . . C17 C 1.9126(3) 0.5665(3) 0.33609(16) 0.0187(9) Uani 1 1 d . . . C18 C 2.0838(3) 0.3791(3) 0.26005(18) 0.0240(10) Uani 1 1 d . . . C21 C 1.6531(3) 0.1473(3) 0.18398(15) 0.0132(9) Uani 1 1 d . . . C22 C 1.6038(3) 0.0464(3) 0.19621(15) 0.0144(9) Uani 1 1 d . . . C23 C 1.5856(3) -0.0305(3) 0.15720(16) 0.0207(10) Uani 1 1 d . . . H23A H 1.5513 -0.1000 0.1643 0.025 Uiso 1 1 calc R . . C24 C 1.6151(3) -0.0104(3) 0.10844(17) 0.0224(10) Uani 1 1 d . . . H24A H 1.6006 -0.0658 0.0830 0.027 Uiso 1 1 calc R . . C25 C 1.6658(3) 0.0904(3) 0.09642(16) 0.0203(10) Uani 1 1 d . . . C26 C 1.6825(3) 0.1688(3) 0.13460(16) 0.0177(9) Uani 1 1 d . . . H26A H 1.7145 0.2380 0.1269 0.021 Uiso 1 1 calc R . . C27 C 1.7060(4) 0.1193(3) 0.04451(17) 0.0250(11) Uani 1 1 d . . . C31 C 1.5012(3) 0.0518(3) 0.26197(15) 0.0127(9) Uani 1 1 d . . . C32 C 1.5692(3) 0.0192(3) 0.24762(15) 0.0149(9) Uani 1 1 d . . . C33 C 1.5932(3) -0.0467(3) 0.27988(16) 0.0177(9) Uani 1 1 d . . . H33A H 1.6394 -0.0703 0.2713 0.021 Uiso 1 1 calc R . . C34 C 1.5504(3) -0.0786(3) 0.32466(17) 0.0204(10) Uani 1 1 d . . . H34A H 1.5678 -0.1239 0.3460 0.024 Uiso 1 1 calc R . . C35 C 1.4828(3) -0.0457(3) 0.33892(16) 0.0173(9) Uani 1 1 d . . . C36 C 1.4580(3) 0.0199(3) 0.30605(15) 0.0155(9) Uani 1 1 d . . . H36A H 1.4108 0.0427 0.3142 0.019 Uiso 1 1 calc R . . C37 C 1.4338(3) -0.0784(3) 0.38742(17) 0.0221(10) Uani 1 1 d . . . C41 C 1.3747(3) 0.0635(3) 0.18649(15) 0.0138(9) Uani 1 1 d . . . C42 C 1.3559(3) 0.1325(3) 0.15366(16) 0.0146(9) Uani 1 1 d . . . C43 C 1.2599(3) 0.0966(3) 0.10954(16) 0.0164(9) Uani 1 1 d . . . C44 C 1.1890(3) -0.0085(3) 0.10295(15) 0.0142(9) Uani 1 1 d . . . H44A H 1.1228 -0.0351 0.0746 0.017 Uiso 1 1 calc R . . C45 C 1.2074(3) -0.0796(3) 0.13532(16) 0.0140(9) Uani 1 1 d . . . C46 C 1.3018(3) -0.0422(3) 0.17749(16) 0.0155(9) Uani 1 1 d . . . H46A H 1.3169 -0.0875 0.2000 0.019 Uiso 1 1 calc R . . C47 C 1.2391(3) 0.1707(3) 0.07342(16) 0.0190(9) Uani 1 1 d . . . C48 C 1.1266(3) -0.1962(3) 0.12544(16) 0.0173(9) Uani 1 1 d . . . C51 C 1.5143(3) 0.4397(3) 0.20857(15) 0.0135(9) Uani 1 1 d . . . C52 C 1.5801(3) 0.4402(3) 0.17562(16) 0.0153(9) Uani 1 1 d . . . C53 C 1.5980(3) 0.5058(3) 0.13446(16) 0.0172(9) Uani 1 1 d . . . C54 C 1.5427(3) 0.5626(3) 0.12756(16) 0.0199(10) Uani 1 1 d . . . H54A H 1.5532 0.6069 0.0999 0.024 Uiso 1 1 calc R . . C55 C 1.4729(3) 0.5586(3) 0.15869(16) 0.0173(9) Uani 1 1 d . . . C56 C 1.4594(3) 0.4950(3) 0.20004(15) 0.0163(9) Uani 1 1 d . . . H56A H 1.4126 0.4900 0.2221 0.020 Uiso 1 1 calc R . . C57 C 1.6746(3) 0.5128(3) 0.09935(17) 0.0191(10) Uani 1 1 d . . . C58 C 1.4083(4) 0.6175(3) 0.14755(17) 0.0242(10) Uani 1 1 d . . . C61 C 1.6024(3) 0.2723(3) 0.36109(16) 0.0147(9) Uani 1 1 d . . . C62 C 1.6022(3) 0.3387(3) 0.40043(16) 0.0157(9) Uani 1 1 d . . . C63 C 1.6667(3) 0.3602(3) 0.45516(15) 0.0159(9) Uani 1 1 d . . . C64 C 1.7371(3) 0.3193(3) 0.46542(16) 0.0191(10) Uani 1 1 d . . . H64A H 1.7818 0.3317 0.5018 0.023 Uiso 1 1 calc R . . C65 C 1.7463(3) 0.2600(3) 0.42459(16) 0.0171(9) Uani 1 1 d . . . C66 C 1.6759(3) 0.2352(3) 0.37243(16) 0.0169(9) Uani 1 1 d . . . H66A H 1.6780 0.1931 0.3447 0.020 Uiso 1 1 calc R . . C67 C 1.6616(3) 0.4282(3) 0.49931(16) 0.0217(10) Uani 1 1 d . . . C68 C 1.8335(3) 0.2259(3) 0.43953(17) 0.0226(10) Uani 1 1 d . . . C71 C 1.2242(3) 0.1568(3) 0.26612(16) 0.0159(9) Uani 1 1 d . . . C72 C 1.2374(3) 0.1604(3) 0.32228(16) 0.0175(9) Uani 1 1 d . . . C73 C 1.1511(3) 0.0941(3) 0.34376(16) 0.0170(9) Uani 1 1 d . . . C74 C 1.0543(3) 0.0280(3) 0.30503(16) 0.0171(9) Uani 1 1 d . . . H74A H 0.9943 -0.0177 0.3182 0.020 Uiso 1 1 calc R . . C75 C 1.0389(3) 0.0239(3) 0.24787(16) 0.0192(10) Uani 1 1 d . . . C76 C 1.1278(3) 0.0894(3) 0.22836(17) 0.0194(10) Uani 1 1 d . . . H76A H 1.1218 0.0876 0.1900 0.023 Uiso 1 1 calc R . . C77 C 1.1631(3) 0.1010(3) 0.40620(16) 0.0189(9) Uani 1 1 d . . . C78 C 0.9249(3) -0.0460(3) 0.20954(17) 0.0219(10) Uani 1 1 d . . . C171 C 2.0315(3) 0.6532(3) 0.3549(2) 0.0341(12) Uani 1 1 d . . . H17A H 2.0758 0.6281 0.3789 0.051 Uiso 1 1 calc R . . H17B H 2.0352 0.7120 0.3751 0.051 Uiso 1 1 calc R . . H17C H 2.0594 0.6750 0.3227 0.051 Uiso 1 1 calc R . . C172 C 1.8461(4) 0.6102(3) 0.29922(18) 0.0328(12) Uani 1 1 d . . . H17D H 1.7693 0.5567 0.2870 0.049 Uiso 1 1 calc R . . H17E H 1.8744 0.6320 0.2671 0.049 Uiso 1 1 calc R . . H17F H 1.8524 0.6695 0.3201 0.049 Uiso 1 1 calc R . . C173 C 1.8710(4) 0.5377(3) 0.38749(17) 0.0311(12) Uani 1 1 d . . . H17G H 1.9129 0.5101 0.4114 0.047 Uiso 1 1 calc R . . H17H H 1.7937 0.4854 0.3765 0.047 Uiso 1 1 calc R . . H17I H 1.8797 0.5993 0.4075 0.047 Uiso 1 1 calc R . . C181 C 2.1811(3) 0.4881(4) 0.2658(2) 0.0382(13) Uani 1 1 d . . . H18A H 2.1929 0.5280 0.3001 0.057 Uiso 1 1 calc R . . H18B H 2.1656 0.5226 0.2346 0.057 Uiso 1 1 calc R . . H18C H 2.2466 0.4832 0.2663 0.057 Uiso 1 1 calc R . . C182 C 2.0679(4) 0.3186(4) 0.20618(19) 0.0384(13) Uani 1 1 d . . . H18D H 2.0063 0.2487 0.2018 0.058 Uiso 1 1 calc R . . H18E H 2.1342 0.3146 0.2073 0.058 Uiso 1 1 calc R . . H18F H 2.0531 0.3537 0.1751 0.058 Uiso 1 1 calc R . . C183 C 2.1124(4) 0.3265(4) 0.3085(2) 0.0402(13) Uani 1 1 d . . . H18G H 2.0515 0.2568 0.3058 0.060 Uiso 1 1 calc R . . H18H H 2.1264 0.3668 0.3431 0.060 Uiso 1 1 calc R . . H18I H 2.1778 0.3223 0.3076 0.060 Uiso 1 1 calc R . . C271 C 1.8302(4) 0.1752(4) 0.0620(2) 0.0409(13) Uani 1 1 d . . . H27A H 1.8557 0.1299 0.0807 0.061 Uiso 1 1 calc R . . H27B H 1.8571 0.2380 0.0872 0.061 Uiso 1 1 calc R . . H27C H 1.8578 0.1936 0.0295 0.061 Uiso 1 1 calc R . . C272 C 1.6653(5) 0.0254(4) 0.0031(2) 0.0518(16) Uani 1 1 d . . . H27D H 1.6908 -0.0211 0.0200 0.078 Uiso 1 1 calc R . . H27E H 1.6935 0.0474 -0.0291 0.078 Uiso 1 1 calc R . . H27F H 1.5854 -0.0108 -0.0085 0.078 Uiso 1 1 calc R . . C273 C 1.6647(4) 0.1900(4) 0.01589(18) 0.0389(13) Uani 1 1 d . . . H27G H 1.6905 0.2079 -0.0172 0.058 Uiso 1 1 calc R . . H27H H 1.6926 0.2531 0.0410 0.058 Uiso 1 1 calc R . . H27I H 1.5848 0.1540 0.0056 0.058 Uiso 1 1 calc R . . C371 C 1.4744(4) -0.1438(4) 0.42146(18) 0.0341(12) Uani 1 1 d . . . H37A H 1.5539 -0.1043 0.4359 0.051 Uiso 1 1 calc R . . H37B H 1.4545 -0.2067 0.3982 0.051 Uiso 1 1 calc R . . H37C H 1.4409 -0.1624 0.4521 0.051 Uiso 1 1 calc R . . C372 C 1.3085(3) -0.1412(4) 0.36560(18) 0.0360(13) Uani 1 1 d . . . H37D H 1.2885 -0.2030 0.3413 0.054 Uiso 1 1 calc R . . H37E H 1.2812 -0.0989 0.3450 0.054 Uiso 1 1 calc R . . H37F H 1.2763 -0.1618 0.3966 0.054 Uiso 1 1 calc R . . C373 C 1.4631(4) 0.0185(3) 0.42546(17) 0.0268(11) Uani 1 1 d . . . H37G H 1.5425 0.0590 0.4400 0.040 Uiso 1 1 calc R . . H37H H 1.4296 -0.0026 0.4560 0.040 Uiso 1 1 calc R . . H37I H 1.4358 0.0605 0.4045 0.040 Uiso 1 1 calc R . . C471 C 1.3357(4) 0.2319(3) 0.04951(17) 0.0293(11) Uani 1 1 d . . . H47A H 1.3454 0.1842 0.0273 0.044 Uiso 1 1 calc R . . H47B H 1.4020 0.2714 0.0796 0.044 Uiso 1 1 calc R . . H47C H 1.3217 0.2794 0.0263 0.044 Uiso 1 1 calc R . . C472 C 1.1355(4) 0.1132(3) 0.02586(17) 0.0321(12) Uani 1 1 d . . . H47D H 1.1432 0.0649 0.0030 0.048 Uiso 1 1 calc R . . H47E H 1.1245 0.1631 0.0035 0.048 Uiso 1 1 calc R . . H47F H 1.0726 0.0750 0.0407 0.048 Uiso 1 1 calc R . . C473 C 1.2248(4) 0.2465(3) 0.10830(18) 0.0280(11) Uani 1 1 d . . . H47G H 1.2904 0.2842 0.1389 0.042 Uiso 1 1 calc R . . H47H H 1.1615 0.2080 0.1228 0.042 Uiso 1 1 calc R . . H47I H 1.2135 0.2955 0.0853 0.042 Uiso 1 1 calc R . . C481 C 1.1024(4) -0.2341(3) 0.17940(18) 0.0331(12) Uani 1 1 d . . . H48A H 1.0689 -0.1985 0.1936 0.050 Uiso 1 1 calc R . . H48B H 1.1705 -0.2195 0.2064 0.050 Uiso 1 1 calc R . . H48C H 1.0522 -0.3086 0.1729 0.050 Uiso 1 1 calc R . . C482 C 1.0186(3) -0.2244(3) 0.08295(18) 0.0269(11) Uani 1 1 d . . . H48D H 0.9836 -0.1890 0.0958 0.040 Uiso 1 1 calc R . . H48E H 0.9704 -0.2992 0.0782 0.040 Uiso 1 1 calc R . . H48F H 1.0328 -0.2031 0.0477 0.040 Uiso 1 1 calc R . . C483 C 1.1790(4) -0.2534(3) 0.10400(19) 0.0303(11) Uani 1 1 d . . . H48G H 1.1282 -0.3278 0.0975 0.045 Uiso 1 1 calc R . . H48H H 1.2465 -0.2393 0.1314 0.045 Uiso 1 1 calc R . . H48I H 1.1956 -0.2295 0.0695 0.045 Uiso 1 1 calc R . . C571 C 1.6289(3) 0.4071(3) 0.06544(16) 0.0241(10) Uani 1 1 d . . . H57A H 1.5565 0.3872 0.0412 0.036 Uiso 1 1 calc R . . H57B H 1.6231 0.3553 0.0903 0.036 Uiso 1 1 calc R . . H57C H 1.6779 0.4116 0.0432 0.036 Uiso 1 1 calc R . . C572 C 1.7890(3) 0.5450(3) 0.13678(17) 0.0265(11) Uani 1 1 d . . . H57D H 1.8181 0.6124 0.1582 0.040 Uiso 1 1 calc R . . H57E H 1.8373 0.5496 0.1142 0.040 Uiso 1 1 calc R . . H57F H 1.7843 0.4936 0.1618 0.040 Uiso 1 1 calc R . . C573 C 1.6869(4) 0.5924(3) 0.05930(18) 0.0299(11) Uani 1 1 d . . . H57G H 1.6152 0.5738 0.0347 0.045 Uiso 1 1 calc R . . H57H H 1.7354 0.5935 0.0375 0.045 Uiso 1 1 calc R . . H57I H 1.7180 0.6608 0.0800 0.045 Uiso 1 1 calc R . . C581 C 1.4372(4) 0.6864(4) 0.10217(18) 0.0358(13) Uani 1 1 d . . . H58A H 1.5147 0.7382 0.1137 0.054 Uiso 1 1 calc R . . H58B H 1.3929 0.7211 0.0957 0.054 Uiso 1 1 calc R . . H58C H 1.4223 0.6439 0.0682 0.054 Uiso 1 1 calc R . . C582 C 1.4321(4) 0.6860(3) 0.20019(17) 0.0287(11) Uani 1 1 d . . . H58D H 1.5096 0.7377 0.2114 0.043 Uiso 1 1 calc R . . H58E H 1.4137 0.6432 0.2296 0.043 Uiso 1 1 calc R . . H58F H 1.3880 0.7208 0.1931 0.043 Uiso 1 1 calc R . . C583 C 1.2862(4) 0.5382(4) 0.1291(2) 0.0369(13) Uani 1 1 d . . . H58G H 1.2665 0.4938 0.1577 0.055 Uiso 1 1 calc R . . H58H H 1.2707 0.4959 0.0949 0.055 Uiso 1 1 calc R . . H58I H 1.2434 0.5744 0.1228 0.055 Uiso 1 1 calc R . . C671 C 1.7318(4) 0.4350(4) 0.55614(17) 0.0323(12) Uani 1 1 d . . . H67A H 1.8079 0.4637 0.5551 0.048 Uiso 1 1 calc R . . H67B H 1.7062 0.3658 0.5673 0.048 Uiso 1 1 calc R . . H67C H 1.7264 0.4797 0.5826 0.048 Uiso 1 1 calc R . . C672 C 1.7017(4) 0.5384(3) 0.48409(17) 0.0287(11) Uani 1 1 d . . . H67D H 1.7775 0.5678 0.4826 0.043 Uiso 1 1 calc R . . H67E H 1.6970 0.5812 0.5119 0.043 Uiso 1 1 calc R . . H67F H 1.6559 0.5363 0.4481 0.043 Uiso 1 1 calc R . . C673 C 1.5424(3) 0.3823(3) 0.50180(17) 0.0292(11) Uani 1 1 d . . . H67G H 1.5170 0.3123 0.5118 0.044 Uiso 1 1 calc R . . H67H H 1.4966 0.3797 0.4657 0.044 Uiso 1 1 calc R . . H67I H 1.5379 0.4256 0.5294 0.044 Uiso 1 1 calc R . . C681 C 1.8154(4) 0.1589(4) 0.4857(2) 0.0469(15) Uani 1 1 d . . . H68A H 1.7444 0.0962 0.4733 0.070 Uiso 1 1 calc R . . H68B H 1.8168 0.1974 0.5178 0.070 Uiso 1 1 calc R . . H68C H 1.8732 0.1400 0.4956 0.070 Uiso 1 1 calc R . . C682 C 1.9469(4) 0.3226(4) 0.4590(2) 0.0456(14) Uani 1 1 d . . . H68D H 2.0030 0.3015 0.4686 0.068 Uiso 1 1 calc R . . H68E H 1.9499 0.3618 0.4913 0.068 Uiso 1 1 calc R . . H68F H 1.9597 0.3659 0.4294 0.068 Uiso 1 1 calc R . . C683 C 1.8344(4) 0.1664(4) 0.39032(19) 0.0405(14) Uani 1 1 d . . . H68G H 1.7642 0.1030 0.3776 0.061 Uiso 1 1 calc R . . H68H H 1.8930 0.1487 0.4013 0.061 Uiso 1 1 calc R . . H68I H 1.8467 0.2093 0.3605 0.061 Uiso 1 1 calc R . . C771 C 1.0598(3) 0.0195(3) 0.41989(17) 0.0297(11) Uani 1 1 d . . . H77A H 1.0705 0.0262 0.4598 0.045 Uiso 1 1 calc R . . H77B H 1.0449 -0.0495 0.4066 0.045 Uiso 1 1 calc R . . H77C H 0.9980 0.0297 0.4020 0.045 Uiso 1 1 calc R . . C772 C 1.1849(4) 0.2080(3) 0.42754(17) 0.0286(11) Uani 1 1 d . . . H77D H 1.1928 0.2130 0.4673 0.043 Uiso 1 1 calc R . . H77E H 1.1238 0.2185 0.4088 0.043 Uiso 1 1 calc R . . H77F H 1.2522 0.2610 0.4202 0.043 Uiso 1 1 calc R . . C773 C 1.2583(3) 0.0835(3) 0.43547(17) 0.0255(11) Uani 1 1 d . . . H77G H 1.2658 0.0880 0.4752 0.038 Uiso 1 1 calc R . . H77H H 1.3258 0.1364 0.4283 0.038 Uiso 1 1 calc R . . H77I H 1.2438 0.0150 0.4216 0.038 Uiso 1 1 calc R . . C781 C 0.8865(4) -0.1584(3) 0.2185(2) 0.0365(13) Uani 1 1 d . . . H78A H 0.8879 -0.1652 0.2573 0.055 Uiso 1 1 calc R . . H78B H 0.9350 -0.1807 0.2086 0.055 Uiso 1 1 calc R . . H78C H 0.8120 -0.2017 0.1954 0.055 Uiso 1 1 calc R . . C782 C 0.9232(4) -0.0369(4) 0.14856(17) 0.0358(13) Uani 1 1 d . . . H78D H 0.9474 0.0350 0.1422 0.054 Uiso 1 1 calc R . . H78E H 0.8488 -0.0808 0.1254 0.054 Uiso 1 1 calc R . . H78F H 0.9722 -0.0591 0.1392 0.054 Uiso 1 1 calc R . . C783 C 0.8441(3) -0.0137(4) 0.22134(19) 0.0307(11) Uani 1 1 d . . . H78G H 0.8436 -0.0180 0.2600 0.046 Uiso 1 1 calc R . . H78H H 0.7709 -0.0599 0.1977 0.046 Uiso 1 1 calc R . . H78I H 0.8665 0.0573 0.2138 0.046 Uiso 1 1 calc R . . C81 C 1.6974(4) -0.2393(4) 0.3148(2) 0.0382(13) Uani 1 1 d . . . H81A H 1.7081 -0.2369 0.2790 0.046 Uiso 1 1 calc R . . C82 C 1.6152(4) -0.3271(4) 0.3268(2) 0.0406(13) Uani 1 1 d . . . H82A H 1.5704 -0.3855 0.2995 0.049 Uiso 1 1 calc R . . C83 C 1.5983(4) -0.3300(4) 0.3783(2) 0.0397(13) Uani 1 1 d . . . H83A H 1.5410 -0.3898 0.3865 0.048 Uiso 1 1 calc R . . C84 C 1.6653(4) -0.2450(4) 0.41804(19) 0.0374(13) Uani 1 1 d . . . H84A H 1.6538 -0.2466 0.4537 0.045 Uiso 1 1 calc R . . C85 C 1.7484(4) -0.1584(4) 0.4064(2) 0.0413(13) Uani 1 1 d . . . H85A H 1.7950 -0.1008 0.4340 0.050 Uiso 1 1 calc R . . C86 C 1.7638(4) -0.1554(4) 0.35467(19) 0.0382(13) Uani 1 1 d . . . H86A H 1.8205 -0.0952 0.3464 0.046 Uiso 1 1 calc R . . C91 C 0.9714(4) -0.4419(4) -0.0361(2) 0.0458(14) Uani 1 1 d . . . H91A H 0.9516 -0.4023 -0.0612 0.055 Uiso 1 1 calc R . . C92 C 0.9131(4) -0.4850(4) 0.0020(2) 0.0443(14) Uani 1 1 d . . . H92A H 0.8538 -0.4742 0.0034 0.053 Uiso 1 1 calc R . . C93 C 0.9409(4) -0.5432(4) 0.0377(2) 0.0466(14) Uani 1 1 d . . . H93A H 0.9003 -0.5733 0.0636 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0133(2) 0.0163(2) 0.01307(19) 0.00374(16) 0.00407(16) 0.00696(17) Mo2 0.0123(2) 0.01271(19) 0.01143(19) 0.00286(15) 0.00259(15) 0.00567(16) O 0.0244(17) 0.0231(16) 0.0209(16) 0.0051(13) 0.0082(13) 0.0169(14) O1 0.0147(16) 0.0161(15) 0.0135(14) 0.0033(12) 0.0054(12) 0.0071(13) O2 0.0152(16) 0.0142(15) 0.0148(15) 0.0049(12) 0.0041(12) 0.0061(13) O11 0.0149(15) 0.0141(15) 0.0133(14) 0.0043(12) 0.0037(12) 0.0081(13) O12 0.0139(15) 0.0170(15) 0.0149(15) 0.0045(12) 0.0033(12) 0.0083(13) O21 0.0141(15) 0.0141(15) 0.0097(14) 0.0029(12) 0.0005(12) 0.0061(13) O22 0.0135(15) 0.0159(15) 0.0160(15) 0.0045(12) 0.0049(12) 0.0067(13) O31 0.0144(16) 0.0205(16) 0.0184(16) 0.0051(13) 0.0053(13) 0.0057(13) O32 0.0138(16) 0.0198(16) 0.0145(15) 0.0017(13) 0.0022(12) 0.0047(13) N1 0.0101(18) 0.0116(17) 0.0132(17) 0.0027(14) 0.0033(14) 0.0028(15) N2 0.0144(19) 0.0143(18) 0.0103(17) 0.0028(14) 0.0025(15) 0.0069(15) C11 0.017(2) 0.015(2) 0.015(2) 0.0090(18) 0.0072(18) 0.0076(19) C12 0.016(2) 0.014(2) 0.012(2) 0.0043(17) 0.0058(18) 0.0090(19) C13 0.017(2) 0.016(2) 0.017(2) 0.0041(18) 0.0049(18) 0.0073(19) C14 0.015(2) 0.019(2) 0.021(2) -0.0012(19) 0.0039(19) 0.005(2) C15 0.016(2) 0.022(2) 0.018(2) 0.0058(19) 0.0054(19) 0.010(2) C16 0.018(2) 0.012(2) 0.016(2) 0.0017(18) 0.0057(19) 0.0050(19) C17 0.014(2) 0.018(2) 0.019(2) -0.0027(19) 0.0025(19) 0.0047(19) C18 0.014(2) 0.025(3) 0.035(3) 0.001(2) 0.006(2) 0.011(2) C21 0.014(2) 0.015(2) 0.013(2) 0.0034(17) 0.0050(17) 0.0077(18) C22 0.015(2) 0.017(2) 0.012(2) 0.0029(17) 0.0008(17) 0.0095(19) C23 0.026(3) 0.015(2) 0.020(2) 0.0016(19) 0.005(2) 0.009(2) C24 0.026(3) 0.021(2) 0.018(2) -0.0014(19) 0.002(2) 0.011(2) C25 0.023(3) 0.022(2) 0.015(2) 0.0031(19) 0.0039(19) 0.011(2) C26 0.014(2) 0.021(2) 0.019(2) 0.0041(19) 0.0068(19) 0.008(2) C27 0.037(3) 0.031(3) 0.015(2) 0.007(2) 0.013(2) 0.020(2) C31 0.010(2) 0.011(2) 0.014(2) 0.0020(17) -0.0014(17) 0.0043(18) C32 0.018(2) 0.013(2) 0.010(2) 0.0001(17) 0.0031(18) 0.0047(19) C33 0.016(2) 0.019(2) 0.019(2) 0.0040(18) 0.0027(19) 0.011(2) C34 0.021(2) 0.019(2) 0.021(2) 0.0068(19) 0.004(2) 0.010(2) C35 0.018(2) 0.017(2) 0.014(2) 0.0042(18) 0.0034(18) 0.007(2) C36 0.009(2) 0.016(2) 0.017(2) -0.0010(18) 0.0017(17) 0.0037(18) C37 0.021(3) 0.028(3) 0.024(2) 0.014(2) 0.010(2) 0.015(2) C41 0.011(2) 0.018(2) 0.011(2) -0.0017(17) 0.0016(17) 0.0060(19) C42 0.014(2) 0.013(2) 0.017(2) 0.0029(17) 0.0093(18) 0.0042(19) C43 0.018(2) 0.016(2) 0.015(2) 0.0033(18) 0.0054(18) 0.0078(19) C44 0.012(2) 0.020(2) 0.010(2) 0.0008(17) 0.0011(17) 0.0083(19) C45 0.014(2) 0.012(2) 0.016(2) 0.0028(17) 0.0047(18) 0.0064(18) C46 0.014(2) 0.013(2) 0.017(2) 0.0031(17) 0.0011(18) 0.0048(18) C47 0.015(2) 0.013(2) 0.021(2) 0.0001(18) -0.0024(19) 0.0038(19) C48 0.015(2) 0.014(2) 0.015(2) -0.0003(18) -0.0012(18) 0.0030(19) C51 0.013(2) 0.015(2) 0.009(2) 0.0026(17) 0.0002(17) 0.0050(18) C52 0.014(2) 0.012(2) 0.015(2) 0.0011(17) 0.0009(18) 0.0038(18) C53 0.018(2) 0.014(2) 0.013(2) 0.0003(17) 0.0026(18) 0.0039(19) C54 0.022(2) 0.017(2) 0.016(2) 0.0066(18) 0.0027(19) 0.007(2) C55 0.022(2) 0.016(2) 0.015(2) 0.0017(18) 0.0019(19) 0.012(2) C56 0.017(2) 0.019(2) 0.013(2) -0.0016(18) 0.0030(18) 0.0091(19) C57 0.022(3) 0.017(2) 0.025(2) 0.0098(19) 0.011(2) 0.012(2) C58 0.034(3) 0.025(3) 0.021(2) 0.006(2) 0.006(2) 0.022(2) C61 0.013(2) 0.012(2) 0.016(2) 0.0039(17) 0.0038(18) 0.0034(18) C62 0.012(2) 0.015(2) 0.017(2) 0.0028(18) 0.0034(18) 0.0041(18) C63 0.013(2) 0.020(2) 0.010(2) 0.0027(18) -0.0001(17) 0.0060(19) C64 0.021(2) 0.021(2) 0.011(2) 0.0054(18) 0.0006(18) 0.009(2) C65 0.015(2) 0.013(2) 0.019(2) 0.0022(18) 0.0019(18) 0.0047(19) C66 0.016(2) 0.014(2) 0.018(2) 0.0056(18) 0.0053(19) 0.0055(19) C67 0.027(3) 0.022(2) 0.013(2) 0.0001(19) 0.0025(19) 0.012(2) C68 0.020(3) 0.027(3) 0.019(2) 0.001(2) -0.0009(19) 0.013(2) C71 0.013(2) 0.018(2) 0.021(2) 0.0049(18) 0.0087(19) 0.0084(19) C72 0.014(2) 0.020(2) 0.018(2) 0.0037(19) 0.0024(19) 0.010(2) C73 0.016(2) 0.022(2) 0.017(2) 0.0074(19) 0.0058(19) 0.011(2) C74 0.015(2) 0.017(2) 0.022(2) 0.0053(18) 0.0098(19) 0.0078(19) C75 0.018(2) 0.021(2) 0.019(2) 0.0008(19) 0.0055(19) 0.009(2) C76 0.022(3) 0.025(2) 0.013(2) -0.0011(19) 0.0033(19) 0.014(2) C77 0.021(2) 0.019(2) 0.017(2) 0.0081(18) 0.0078(19) 0.009(2) C78 0.013(2) 0.023(2) 0.021(2) -0.002(2) 0.0036(19) 0.003(2) C171 0.022(3) 0.023(3) 0.046(3) -0.010(2) 0.009(2) 0.002(2) C172 0.042(3) 0.028(3) 0.032(3) 0.006(2) 0.004(2) 0.022(3) C173 0.035(3) 0.021(3) 0.023(3) -0.002(2) 0.008(2) 0.003(2) C181 0.017(3) 0.035(3) 0.061(4) 0.001(3) 0.016(3) 0.010(2) C182 0.022(3) 0.048(3) 0.050(3) -0.003(3) 0.016(2) 0.017(3) C183 0.031(3) 0.051(3) 0.049(3) 0.018(3) 0.009(3) 0.028(3) C271 0.030(3) 0.056(4) 0.036(3) 0.018(3) 0.017(2) 0.017(3) C272 0.076(4) 0.051(4) 0.033(3) -0.002(3) 0.034(3) 0.025(3) C273 0.052(4) 0.058(4) 0.026(3) 0.019(3) 0.018(3) 0.038(3) C371 0.049(3) 0.036(3) 0.028(3) 0.017(2) 0.017(2) 0.025(3) C372 0.026(3) 0.042(3) 0.029(3) 0.012(2) 0.012(2) 0.005(2) C373 0.030(3) 0.038(3) 0.020(2) 0.010(2) 0.010(2) 0.022(2) C471 0.035(3) 0.022(3) 0.022(2) 0.012(2) 0.003(2) 0.009(2) C472 0.034(3) 0.026(3) 0.026(3) 0.007(2) -0.008(2) 0.014(2) C473 0.031(3) 0.024(3) 0.028(3) 0.009(2) 0.001(2) 0.017(2) C481 0.025(3) 0.026(3) 0.033(3) 0.006(2) 0.006(2) 0.001(2) C482 0.015(2) 0.018(2) 0.034(3) 0.002(2) -0.005(2) 0.003(2) C483 0.026(3) 0.023(3) 0.039(3) -0.002(2) 0.004(2) 0.011(2) C571 0.026(3) 0.028(3) 0.019(2) 0.005(2) 0.011(2) 0.012(2) C572 0.018(3) 0.028(3) 0.030(3) 0.006(2) 0.013(2) 0.005(2) C573 0.036(3) 0.032(3) 0.032(3) 0.019(2) 0.019(2) 0.021(2) C581 0.058(4) 0.043(3) 0.029(3) 0.013(2) 0.011(3) 0.043(3) C582 0.039(3) 0.028(3) 0.030(3) 0.007(2) 0.009(2) 0.024(2) C583 0.032(3) 0.033(3) 0.046(3) 0.001(2) -0.001(2) 0.020(3) C671 0.032(3) 0.042(3) 0.021(3) -0.002(2) 0.000(2) 0.020(3) C672 0.036(3) 0.021(3) 0.022(3) -0.004(2) 0.005(2) 0.010(2) C673 0.037(3) 0.035(3) 0.022(3) 0.008(2) 0.015(2) 0.019(2) C681 0.052(4) 0.056(4) 0.054(4) 0.032(3) 0.020(3) 0.041(3) C682 0.021(3) 0.043(3) 0.065(4) -0.003(3) -0.002(3) 0.015(3) C683 0.038(3) 0.059(4) 0.037(3) -0.007(3) -0.004(2) 0.040(3) C771 0.024(3) 0.039(3) 0.020(2) 0.008(2) 0.011(2) 0.008(2) C772 0.033(3) 0.034(3) 0.024(3) 0.008(2) 0.011(2) 0.019(2) C773 0.031(3) 0.030(3) 0.023(2) 0.010(2) 0.013(2) 0.019(2) C781 0.025(3) 0.025(3) 0.049(3) -0.008(2) 0.006(2) 0.005(2) C782 0.022(3) 0.052(3) 0.021(3) -0.003(2) 0.001(2) 0.011(3) C783 0.016(3) 0.035(3) 0.037(3) 0.000(2) 0.003(2) 0.011(2) C81 0.036(3) 0.053(4) 0.028(3) 0.007(3) 0.009(2) 0.024(3) C82 0.046(3) 0.037(3) 0.028(3) -0.001(2) 0.007(3) 0.013(3) C83 0.036(3) 0.033(3) 0.035(3) 0.008(2) 0.003(3) 0.008(3) C84 0.038(3) 0.040(3) 0.026(3) 0.007(2) 0.009(2) 0.012(3) C85 0.035(3) 0.042(3) 0.033(3) 0.000(3) 0.004(3) 0.011(3) C86 0.021(3) 0.053(4) 0.032(3) 0.012(3) 0.005(2) 0.012(3) C91 0.040(3) 0.040(3) 0.050(4) 0.004(3) 0.003(3) 0.017(3) C92 0.038(3) 0.041(3) 0.049(4) -0.003(3) 0.016(3) 0.013(3) C93 0.044(4) 0.043(3) 0.047(4) 0.000(3) 0.013(3) 0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O 1.683(3) . ? Mo1 O22 1.930(3) . ? Mo1 O31 1.948(3) . ? Mo1 O32 1.954(3) . ? Mo1 O11 2.042(2) . ? Mo1 O21 2.215(3) . ? Mo2 O12 1.987(3) . ? Mo2 O1 2.008(3) . ? Mo2 N1 2.015(3) . ? Mo2 O2 2.027(3) . ? Mo2 N2 2.039(3) . ? Mo2 O21 2.146(2) . ? Mo2 O11 2.159(2) . ? O1 C12 1.319(4) . ? O2 C42 1.315(4) . ? O11 C51 1.392(4) . ? O12 C52 1.353(4) . ? O21 C61 1.359(4) . ? O22 C62 1.348(4) . ? O31 C71 1.370(4) . ? O32 C72 1.373(4) . ? N1 C11 1.381(5) . ? N1 C21 1.441(5) . ? N2 C41 1.379(5) . ? N2 C31 1.432(5) . ? C11 C16 1.409(5) . ? C11 C12 1.422(5) . ? C12 C13 1.412(5) . ? C13 C14 1.388(5) . ? C13 C17 1.524(5) . ? C14 C15 1.423(5) . ? C14 H14A 0.9500 . ? C15 C16 1.380(5) . ? C15 C18 1.536(5) . ? C16 H16A 0.9500 . ? C17 C173 1.534(5) . ? C17 C171 1.534(5) . ? C17 C172 1.542(6) . ? C18 C183 1.532(6) . ? C18 C182 1.535(6) . ? C18 C181 1.538(6) . ? C21 C22 1.394(5) . ? C21 C26 1.399(5) . ? C22 C23 1.386(5) . ? C22 C32 1.487(5) . ? C23 C24 1.383(5) . ? C23 H23A 0.9500 . ? C24 C25 1.392(5) . ? C24 H24A 0.9500 . ? C25 C26 1.398(5) . ? C25 C27 1.536(5) . ? C26 H26A 0.9500 . ? C27 C272 1.519(6) . ? C27 C271 1.523(6) . ? C27 C273 1.538(6) . ? C31 C36 1.378(5) . ? C31 C32 1.392(5) . ? C32 C33 1.389(5) . ? C33 C34 1.392(5) . ? C33 H33A 0.9500 . ? C34 C35 1.388(5) . ? C34 H34A 0.9500 . ? C35 C36 1.399(5) . ? C35 C37 1.523(5) . ? C36 H36A 0.9500 . ? C37 C371 1.526(5) . ? C37 C372 1.542(6) . ? C37 C373 1.545(6) . ? C41 C46 1.394(5) . ? C41 C42 1.404(5) . ? C42 C43 1.420(5) . ? C43 C44 1.384(5) . ? C43 C47 1.523(5) . ? C44 C45 1.421(5) . ? C44 H44A 0.9500 . ? C45 C46 1.378(5) . ? C45 C48 1.539(5) . ? C46 H46A 0.9500 . ? C47 C471 1.529(5) . ? C47 C472 1.532(5) . ? C47 C473 1.541(6) . ? C48 C481 1.528(5) . ? C48 C482 1.534(5) . ? C48 C483 1.542(5) . ? C51 C56 1.371(5) . ? C51 C52 1.398(5) . ? C52 C53 1.410(5) . ? C53 C54 1.395(5) . ? C53 C57 1.539(5) . ? C54 C55 1.396(5) . ? C54 H54A 0.9500 . ? C55 C56 1.395(5) . ? C55 C58 1.535(5) . ? C56 H56A 0.9500 . ? C57 C573 1.530(5) . ? C57 C572 1.538(6) . ? C57 C571 1.540(5) . ? C58 C581 1.536(6) . ? C58 C582 1.536(6) . ? C58 C583 1.538(6) . ? C61 C66 1.385(5) . ? C61 C62 1.397(5) . ? C62 C63 1.410(5) . ? C63 C64 1.387(5) . ? C63 C67 1.537(5) . ? C64 C65 1.421(5) . ? C64 H64A 0.9500 . ? C65 C66 1.384(5) . ? C65 C68 1.536(5) . ? C66 H66A 0.9500 . ? C67 C671 1.520(5) . ? C67 C672 1.539(6) . ? C67 C673 1.541(6) . ? C68 C681 1.523(6) . ? C68 C683 1.526(6) . ? C68 C682 1.542(6) . ? C71 C76 1.379(5) . ? C71 C72 1.382(5) . ? C72 C73 1.406(5) . ? C73 C74 1.388(5) . ? C73 C77 1.541(5) . ? C74 C75 1.403(5) . ? C74 H74A 0.9500 . ? C75 C76 1.398(5) . ? C75 C78 1.535(5) . ? C76 H76A 0.9500 . ? C77 C771 1.532(5) . ? C77 C772 1.533(6) . ? C77 C773 1.536(5) . ? C78 C781 1.526(6) . ? C78 C783 1.537(6) . ? C78 C782 1.540(6) . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? C173 H17G 0.9800 . ? C173 H17H 0.9800 . ? C173 H17I 0.9800 . ? C181 H18A 0.9800 . ? C181 H18B 0.9800 . ? C181 H18C 0.9800 . ? C182 H18D 0.9800 . ? C182 H18E 0.9800 . ? C182 H18F 0.9800 . ? C183 H18G 0.9800 . ? C183 H18H 0.9800 . ? C183 H18I 0.9800 . ? C271 H27A 0.9800 . ? C271 H27B 0.9800 . ? C271 H27C 0.9800 . ? C272 H27D 0.9800 . ? C272 H27E 0.9800 . ? C272 H27F 0.9800 . ? C273 H27G 0.9800 . ? C273 H27H 0.9800 . ? C273 H27I 0.9800 . ? C371 H37A 0.9800 . ? C371 H37B 0.9800 . ? C371 H37C 0.9800 . ? C372 H37D 0.9800 . ? C372 H37E 0.9800 . ? C372 H37F 0.9800 . ? C373 H37G 0.9800 . ? C373 H37H 0.9800 . ? C373 H37I 0.9800 . ? C471 H47A 0.9800 . ? C471 H47B 0.9800 . ? C471 H47C 0.9800 . ? C472 H47D 0.9800 . ? C472 H47E 0.9800 . ? C472 H47F 0.9800 . ? C473 H47G 0.9800 . ? C473 H47H 0.9800 . ? C473 H47I 0.9800 . ? C481 H48A 0.9800 . ? C481 H48B 0.9800 . ? C481 H48C 0.9800 . ? C482 H48D 0.9800 . ? C482 H48E 0.9800 . ? C482 H48F 0.9800 . ? C483 H48G 0.9800 . ? C483 H48H 0.9800 . ? C483 H48I 0.9800 . ? C571 H57A 0.9800 . ? C571 H57B 0.9800 . ? C571 H57C 0.9800 . ? C572 H57D 0.9800 . ? C572 H57E 0.9800 . ? C572 H57F 0.9800 . ? C573 H57G 0.9800 . ? C573 H57H 0.9800 . ? C573 H57I 0.9800 . ? C581 H58A 0.9800 . ? C581 H58B 0.9800 . ? C581 H58C 0.9800 . ? C582 H58D 0.9800 . ? C582 H58E 0.9800 . ? C582 H58F 0.9800 . ? C583 H58G 0.9800 . ? C583 H58H 0.9800 . ? C583 H58I 0.9800 . ? C671 H67A 0.9800 . ? C671 H67B 0.9800 . ? C671 H67C 0.9800 . ? C672 H67D 0.9800 . ? C672 H67E 0.9800 . ? C672 H67F 0.9800 . ? C673 H67G 0.9800 . ? C673 H67H 0.9800 . ? C673 H67I 0.9800 . ? C681 H68A 0.9800 . ? C681 H68B 0.9800 . ? C681 H68C 0.9800 . ? C682 H68D 0.9800 . ? C682 H68E 0.9800 . ? C682 H68F 0.9800 . ? C683 H68G 0.9800 . ? C683 H68H 0.9800 . ? C683 H68I 0.9800 . ? C771 H77A 0.9800 . ? C771 H77B 0.9800 . ? C771 H77C 0.9800 . ? C772 H77D 0.9800 . ? C772 H77E 0.9800 . ? C772 H77F 0.9800 . ? C773 H77G 0.9800 . ? C773 H77H 0.9800 . ? C773 H77I 0.9800 . ? C781 H78A 0.9800 . ? C781 H78B 0.9800 . ? C781 H78C 0.9800 . ? C782 H78D 0.9800 . ? C782 H78E 0.9800 . ? C782 H78F 0.9800 . ? C783 H78G 0.9800 . ? C783 H78H 0.9800 . ? C783 H78I 0.9800 . ? C81 C86 1.374(6) . ? C81 C82 1.382(6) . ? C81 H81A 0.9500 . ? C82 C83 1.373(6) . ? C82 H82A 0.9500 . ? C83 C84 1.383(6) . ? C83 H83A 0.9500 . ? C84 C85 1.375(6) . ? C84 H84A 0.9500 . ? C85 C86 1.371(6) . ? C85 H85A 0.9500 . ? C86 H86A 0.9500 . ? C91 C92 1.385(7) . ? C91 C93 1.392(7) 2_745 ? C91 H91A 0.9500 . ? C92 C93 1.371(7) . ? C92 H92A 0.9500 . ? C93 C91 1.392(7) 2_745 ? C93 H93A 0.9500 . ? 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 O Mo1 O22 94.36(12) . . ? O Mo1 O31 104.96(12) . . ? O22 Mo1 O31 156.98(11) . . ? O Mo1 O32 103.50(12) . . ? O22 Mo1 O32 85.23(11) . . ? O31 Mo1 O32 78.25(11) . . ? O Mo1 O11 95.42(11) . . ? O22 Mo1 O11 107.15(10) . . ? O31 Mo1 O11 83.72(10) . . ? O32 Mo1 O11 156.60(11) . . ? O Mo1 O21 158.35(12) . . ? O22 Mo1 O21 74.15(10) . . ? O31 Mo1 O21 90.95(10) . . ? O32 Mo1 O21 93.93(10) . . ? O11 Mo1 O21 71.43(9) . . ? O12 Mo2 O1 80.66(10) . . ? O12 Mo2 N1 84.92(11) . . ? O1 Mo2 N1 76.14(11) . . ? O12 Mo2 O2 78.04(10) . . ? O1 Mo2 O2 154.90(10) . . ? N1 Mo2 O2 114.71(11) . . ? O12 Mo2 N2 139.49(11) . . ? O1 Mo2 N2 132.31(11) . . ? N1 Mo2 N2 82.58(12) . . ? O2 Mo2 N2 72.70(11) . . ? O12 Mo2 O21 141.11(10) . . ? O1 Mo2 O21 74.90(10) . . ? N1 Mo2 O21 117.06(11) . . ? O2 Mo2 O21 115.06(10) . . ? N2 Mo2 O21 77.89(11) . . ? O12 Mo2 O11 76.90(10) . . ? O1 Mo2 O11 83.23(10) . . ? N1 Mo2 O11 154.45(11) . . ? O2 Mo2 O11 79.15(10) . . ? N2 Mo2 O11 122.82(11) . . ? O21 Mo2 O11 70.63(9) . . ? C12 O1 Mo2 117.0(2) . . ? C42 O2 Mo2 122.6(2) . . ? C51 O11 Mo1 137.0(2) . . ? C51 O11 Mo2 110.7(2) . . ? Mo1 O11 Mo2 109.52(11) . . ? C52 O12 Mo2 116.1(2) . . ? C61 O21 Mo2 125.1(2) . . ? C61 O21 Mo1 113.0(2) . . ? Mo2 O21 Mo1 103.80(10) . . ? C62 O22 Mo1 122.5(2) . . ? C71 O31 Mo1 117.2(2) . . ? C72 O32 Mo1 117.1(2) . . ? C11 N1 C21 117.6(3) . . ? C11 N1 Mo2 116.2(3) . . ? C21 N1 Mo2 124.6(2) . . ? C41 N2 C31 115.6(3) . . ? C41 N2 Mo2 120.7(2) . . ? C31 N2 Mo2 123.5(2) . . ? N1 C11 C16 127.6(4) . . ? N1 C11 C12 112.0(3) . . ? C16 C11 C12 120.4(4) . . ? O1 C12 C13 124.8(3) . . ? O1 C12 C11 114.0(3) . . ? C13 C12 C11 121.1(4) . . ? C14 C13 C12 115.6(4) . . ? C14 C13 C17 122.8(4) . . ? C12 C13 C17 121.5(3) . . ? C13 C14 C15 124.7(4) . . ? C13 C14 H14A 117.7 . . ? C15 C14 H14A 117.7 . . ? C16 C15 C14 118.3(4) . . ? C16 C15 C18 121.5(4) . . ? C14 C15 C18 120.0(4) . . ? C15 C16 C11 119.6(4) . . ? C15 C16 H16A 120.2 . . ? C11 C16 H16A 120.2 . . ? C13 C17 C173 111.1(3) . . ? C13 C17 C171 112.5(3) . . ? C173 C17 C171 107.7(3) . . ? C13 C17 C172 109.2(3) . . ? C173 C17 C172 108.7(4) . . ? C171 C17 C172 107.5(4) . . ? C183 C18 C182 109.1(4) . . ? C183 C18 C15 108.1(3) . . ? C182 C18 C15 112.0(3) . . ? C183 C18 C181 107.9(4) . . ? C182 C18 C181 108.2(4) . . ? C15 C18 C181 111.5(3) . . ? C22 C21 C26 120.9(4) . . ? C22 C21 N1 120.6(3) . . ? C26 C21 N1 118.5(3) . . ? C23 C22 C21 116.8(4) . . ? C23 C22 C32 120.2(4) . . ? C21 C22 C32 123.0(3) . . ? C24 C23 C22 123.0(4) . . ? C24 C23 H23A 118.5 . . ? C22 C23 H23A 118.5 . . ? C23 C24 C25 120.4(4) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C24 C25 C26 117.5(4) . . ? C24 C25 C27 123.5(4) . . ? C26 C25 C27 119.0(4) . . ? C25 C26 C21 121.3(4) . . ? C25 C26 H26A 119.3 . . ? C21 C26 H26A 119.3 . . ? C272 C27 C271 109.1(4) . . ? C272 C27 C25 112.4(4) . . ? C271 C27 C25 107.9(4) . . ? C272 C27 C273 107.4(4) . . ? C271 C27 C273 110.1(4) . . ? C25 C27 C273 109.9(3) . . ? C36 C31 C32 122.0(4) . . ? C36 C31 N2 119.9(3) . . ? C32 C31 N2 118.1(3) . . ? C33 C32 C31 117.4(4) . . ? C33 C32 C22 122.4(4) . . ? C31 C32 C22 119.9(3) . . ? C32 C33 C34 120.9(4) . . ? C32 C33 H33A 119.5 . . ? C34 C33 H33A 119.5 . . ? C35 C34 C33 121.6(4) . . ? C35 C34 H34A 119.2 . . ? C33 C34 H34A 119.2 . . ? C34 C35 C36 117.4(4) . . ? C34 C35 C37 123.7(4) . . ? C36 C35 C37 118.9(4) . . ? C31 C36 C35 120.8(4) . . ? C31 C36 H36A 119.6 . . ? C35 C36 H36A 119.6 . . ? C35 C37 C371 112.7(3) . . ? C35 C37 C372 109.0(3) . . ? C371 C37 C372 108.8(4) . . ? C35 C37 C373 109.6(3) . . ? C371 C37 C373 108.4(3) . . ? C372 C37 C373 108.4(4) . . ? N2 C41 C46 127.0(4) . . ? N2 C41 C42 110.7(3) . . ? C46 C41 C42 122.3(4) . . ? O2 C42 C41 113.1(3) . . ? O2 C42 C43 126.2(4) . . ? C41 C42 C43 120.7(4) . . ? C44 C43 C42 115.0(4) . . ? C44 C43 C47 124.0(4) . . ? C42 C43 C47 121.1(3) . . ? C43 C44 C45 125.1(4) . . ? C43 C44 H44A 117.4 . . ? C45 C44 H44A 117.4 . . ? C46 C45 C44 118.3(4) . . ? C46 C45 C48 118.7(3) . . ? C44 C45 C48 123.0(3) . . ? C45 C46 C41 118.6(4) . . ? C45 C46 H46A 120.7 . . ? C41 C46 H46A 120.7 . . ? C43 C47 C471 109.9(3) . . ? C43 C47 C472 111.6(3) . . ? C471 C47 C472 108.7(3) . . ? C43 C47 C473 109.4(3) . . ? C471 C47 C473 109.0(3) . . ? C472 C47 C473 108.2(3) . . ? C481 C48 C482 108.7(3) . . ? C481 C48 C45 110.1(3) . . ? C482 C48 C45 112.8(3) . . ? C481 C48 C483 108.5(4) . . ? C482 C48 C483 108.0(3) . . ? C45 C48 C483 108.7(3) . . ? C56 C51 O11 124.0(3) . . ? C56 C51 C52 122.7(4) . . ? O11 C51 C52 113.4(3) . . ? O12 C52 C51 117.7(3) . . ? O12 C52 C53 123.0(4) . . ? C51 C52 C53 119.3(4) . . ? C54 C53 C52 116.5(4) . . ? C54 C53 C57 122.6(3) . . ? C52 C53 C57 120.9(4) . . ? C53 C54 C55 124.3(4) . . ? C53 C54 H54A 117.8 . . ? C55 C54 H54A 117.8 . . ? C56 C55 C54 117.6(4) . . ? C56 C55 C58 119.7(4) . . ? C54 C55 C58 122.7(4) . . ? C51 C56 C55 119.5(4) . . ? C51 C56 H56A 120.3 . . ? C55 C56 H56A 120.3 . . ? C573 C57 C572 107.5(3) . . ? C573 C57 C53 112.3(3) . . ? C572 C57 C53 109.9(3) . . ? C573 C57 C571 108.0(3) . . ? C572 C57 C571 109.6(3) . . ? C53 C57 C571 109.6(3) . . ? C55 C58 C581 112.1(3) . . ? C55 C58 C582 110.1(3) . . ? C581 C58 C582 108.4(4) . . ? C55 C58 C583 108.2(3) . . ? C581 C58 C583 108.6(4) . . ? C582 C58 C583 109.5(4) . . ? O21 C61 C66 125.1(4) . . ? O21 C61 C62 113.7(3) . . ? C66 C61 C62 121.1(4) . . ? O22 C62 C61 114.3(3) . . ? O22 C62 C63 124.1(4) . . ? C61 C62 C63 121.4(4) . . ? C64 C63 C62 115.5(4) . . ? C64 C63 C67 123.0(3) . . ? C62 C63 C67 121.5(4) . . ? C63 C64 C65 123.8(4) . . ? C63 C64 H64A 118.1 . . ? C65 C64 H64A 118.1 . . ? C66 C65 C64 118.4(4) . . ? C66 C65 C68 122.3(4) . . ? C64 C65 C68 119.3(3) . . ? C65 C66 C61 119.3(4) . . ? C65 C66 H66A 120.4 . . ? C61 C66 H66A 120.4 . . ? C671 C67 C63 112.7(3) . . ? C671 C67 C672 107.9(4) . . ? C63 C67 C672 109.7(3) . . ? C671 C67 C673 108.6(3) . . ? C63 C67 C673 108.6(3) . . ? C672 C67 C673 109.3(4) . . ? C681 C68 C683 109.0(4) . . ? C681 C68 C65 110.6(4) . . ? C683 C68 C65 112.2(3) . . ? C681 C68 C682 108.8(4) . . ? C683 C68 C682 107.2(4) . . ? C65 C68 C682 108.9(4) . . ? O31 C71 C76 123.7(4) . . ? O31 C71 C72 113.4(4) . . ? C76 C71 C72 122.8(4) . . ? O32 C72 C71 113.0(3) . . ? O32 C72 C73 126.2(4) . . ? C71 C72 C73 120.7(4) . . ? C74 C73 C72 115.5(4) . . ? C74 C73 C77 123.2(3) . . ? C72 C73 C77 121.2(4) . . ? C73 C74 C75 124.6(4) . . ? C73 C74 H74A 117.7 . . ? C75 C74 H74A 117.7 . . ? C76 C75 C74 117.9(4) . . ? C76 C75 C78 122.7(4) . . ? C74 C75 C78 119.3(4) . . ? C71 C76 C75 118.4(4) . . ? C71 C76 H76A 120.8 . . ? C75 C76 H76A 120.8 . . ? C771 C77 C772 108.4(3) . . ? C771 C77 C773 108.0(3) . . ? C772 C77 C773 109.9(3) . . ? C771 C77 C73 111.8(3) . . ? C772 C77 C73 109.1(3) . . ? C773 C77 C73 109.6(3) . . ? C781 C78 C75 110.3(4) . . ? C781 C78 C783 109.3(3) . . ? C75 C78 C783 109.6(3) . . ? C781 C78 C782 108.7(4) . . ? C75 C78 C782 111.8(3) . . ? C783 C78 C782 107.2(4) . . ? C17 C171 H17A 109.5 . . ? C17 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C17 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C17 C172 H17D 109.5 . . ? C17 C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? C17 C172 H17F 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? C17 C173 H17G 109.5 . . ? C17 C173 H17H 109.5 . . ? H17G C173 H17H 109.5 . . ? C17 C173 H17I 109.5 . . ? H17G C173 H17I 109.5 . . ? H17H C173 H17I 109.5 . . ? C18 C181 H18A 109.5 . . ? C18 C181 H18B 109.5 . . ? H18A C181 H18B 109.5 . . ? C18 C181 H18C 109.5 . . ? H18A C181 H18C 109.5 . . ? H18B C181 H18C 109.5 . . ? C18 C182 H18D 109.5 . . ? C18 C182 H18E 109.5 . . ? H18D C182 H18E 109.5 . . ? C18 C182 H18F 109.5 . . ? H18D C182 H18F 109.5 . . ? H18E C182 H18F 109.5 . . ? C18 C183 H18G 109.5 . . ? C18 C183 H18H 109.5 . . ? H18G C183 H18H 109.5 . . ? C18 C183 H18I 109.5 . . ? H18G C183 H18I 109.5 . . ? H18H C183 H18I 109.5 . . ? C27 C271 H27A 109.5 . . ? C27 C271 H27B 109.5 . . ? H27A C271 H27B 109.5 . . ? C27 C271 H27C 109.5 . . ? H27A C271 H27C 109.5 . . ? H27B C271 H27C 109.5 . . ? C27 C272 H27D 109.5 . . ? C27 C272 H27E 109.5 . . ? H27D C272 H27E 109.5 . . ? C27 C272 H27F 109.5 . . ? H27D C272 H27F 109.5 . . ? H27E C272 H27F 109.5 . . ? C27 C273 H27G 109.5 . . ? C27 C273 H27H 109.5 . . ? H27G C273 H27H 109.5 . . ? C27 C273 H27I 109.5 . . ? H27G C273 H27I 109.5 . . ? H27H C273 H27I 109.5 . . ? C37 C371 H37A 109.5 . . ? C37 C371 H37B 109.5 . . ? H37A C371 H37B 109.5 . . ? C37 C371 H37C 109.5 . . ? H37A C371 H37C 109.5 . . ? H37B C371 H37C 109.5 . . ? C37 C372 H37D 109.5 . . ? C37 C372 H37E 109.5 . . ? H37D C372 H37E 109.5 . . ? C37 C372 H37F 109.5 . . ? H37D C372 H37F 109.5 . . ? H37E C372 H37F 109.5 . . ? C37 C373 H37G 109.5 . . ? C37 C373 H37H 109.5 . . ? H37G C373 H37H 109.5 . . ? C37 C373 H37I 109.5 . . ? H37G C373 H37I 109.5 . . ? H37H C373 H37I 109.5 . . ? C47 C471 H47A 109.5 . . ? C47 C471 H47B 109.5 . . ? H47A C471 H47B 109.5 . . ? C47 C471 H47C 109.5 . . ? H47A C471 H47C 109.5 . . ? H47B C471 H47C 109.5 . . ? C47 C472 H47D 109.5 . . ? C47 C472 H47E 109.5 . . ? H47D C472 H47E 109.5 . . ? C47 C472 H47F 109.5 . . ? H47D C472 H47F 109.5 . . ? H47E C472 H47F 109.5 . . ? C47 C473 H47G 109.5 . . ? C47 C473 H47H 109.5 . . ? H47G C473 H47H 109.5 . . ? C47 C473 H47I 109.5 . . ? H47G C473 H47I 109.5 . . ? H47H C473 H47I 109.5 . . ? C48 C481 H48A 109.5 . . ? C48 C481 H48B 109.5 . . ? H48A C481 H48B 109.5 . . ? C48 C481 H48C 109.5 . . ? H48A C481 H48C 109.5 . . ? H48B C481 H48C 109.5 . . ? C48 C482 H48D 109.5 . . ? C48 C482 H48E 109.5 . . ? H48D C482 H48E 109.5 . . ? C48 C482 H48F 109.5 . . ? H48D C482 H48F 109.5 . . ? H48E C482 H48F 109.5 . . ? C48 C483 H48G 109.5 . . ? C48 C483 H48H 109.5 . . ? H48G C483 H48H 109.5 . . ? C48 C483 H48I 109.5 . . ? H48G C483 H48I 109.5 . . ? H48H C483 H48I 109.5 . . ? C57 C571 H57A 109.5 . . ? C57 C571 H57B 109.5 . . ? H57A C571 H57B 109.5 . . ? C57 C571 H57C 109.5 . . ? H57A C571 H57C 109.5 . . ? H57B C571 H57C 109.5 . . ? C57 C572 H57D 109.5 . . ? C57 C572 H57E 109.5 . . ? H57D C572 H57E 109.5 . . ? C57 C572 H57F 109.5 . . ? H57D C572 H57F 109.5 . . ? H57E C572 H57F 109.5 . . ? C57 C573 H57G 109.5 . . ? C57 C573 H57H 109.5 . . ? H57G C573 H57H 109.5 . . ? C57 C573 H57I 109.5 . . ? H57G C573 H57I 109.5 . . ? H57H C573 H57I 109.5 . . ? C58 C581 H58A 109.5 . . ? C58 C581 H58B 109.5 . . ? H58A C581 H58B 109.5 . . ? C58 C581 H58C 109.5 . . ? H58A C581 H58C 109.5 . . ? H58B C581 H58C 109.5 . . ? C58 C582 H58D 109.5 . . ? C58 C582 H58E 109.5 . . ? H58D C582 H58E 109.5 . . ? C58 C582 H58F 109.5 . . ? H58D C582 H58F 109.5 . . ? H58E C582 H58F 109.5 . . ? C58 C583 H58G 109.5 . . ? C58 C583 H58H 109.5 . . ? H58G C583 H58H 109.5 . . ? C58 C583 H58I 109.5 . . ? H58G C583 H58I 109.5 . . ? H58H C583 H58I 109.5 . . ? C67 C671 H67A 109.5 . . ? C67 C671 H67B 109.5 . . ? H67A C671 H67B 109.5 . . ? C67 C671 H67C 109.5 . . ? H67A C671 H67C 109.5 . . ? H67B C671 H67C 109.5 . . ? C67 C672 H67D 109.5 . . ? C67 C672 H67E 109.5 . . ? H67D C672 H67E 109.5 . . ? C67 C672 H67F 109.5 . . ? H67D C672 H67F 109.5 . . ? H67E C672 H67F 109.5 . . ? C67 C673 H67G 109.5 . . ? C67 C673 H67H 109.5 . . ? H67G C673 H67H 109.5 . . ? C67 C673 H67I 109.5 . . ? H67G C673 H67I 109.5 . . ? H67H C673 H67I 109.5 . . ? C68 C681 H68A 109.5 . . ? C68 C681 H68B 109.5 . . ? H68A C681 H68B 109.5 . . ? C68 C681 H68C 109.5 . . ? H68A C681 H68C 109.5 . . ? H68B C681 H68C 109.5 . . ? C68 C682 H68D 109.5 . . ? C68 C682 H68E 109.5 . . ? H68D C682 H68E 109.5 . . ? C68 C682 H68F 109.5 . . ? H68D C682 H68F 109.5 . . ? H68E C682 H68F 109.5 . . ? C68 C683 H68G 109.5 . . ? C68 C683 H68H 109.5 . . ? H68G C683 H68H 109.5 . . ? C68 C683 H68I 109.5 . . ? H68G C683 H68I 109.5 . . ? H68H C683 H68I 109.5 . . ? C77 C771 H77A 109.5 . . ? C77 C771 H77B 109.5 . . ? H77A C771 H77B 109.5 . . ? C77 C771 H77C 109.5 . . ? H77A C771 H77C 109.5 . . ? H77B C771 H77C 109.5 . . ? C77 C772 H77D 109.5 . . ? C77 C772 H77E 109.5 . . ? H77D C772 H77E 109.5 . . ? C77 C772 H77F 109.5 . . ? H77D C772 H77F 109.5 . . ? H77E C772 H77F 109.5 . . ? C77 C773 H77G 109.5 . . ? C77 C773 H77H 109.5 . . ? H77G C773 H77H 109.5 . . ? C77 C773 H77I 109.5 . . ? H77G C773 H77I 109.5 . . ? H77H C773 H77I 109.5 . . ? C78 C781 H78A 109.5 . . ? C78 C781 H78B 109.5 . . ? H78A C781 H78B 109.5 . . ? C78 C781 H78C 109.5 . . ? H78A C781 H78C 109.5 . . ? H78B C781 H78C 109.5 . . ? C78 C782 H78D 109.5 . . ? C78 C782 H78E 109.5 . . ? H78D C782 H78E 109.5 . . ? C78 C782 H78F 109.5 . . ? H78D C782 H78F 109.5 . . ? H78E C782 H78F 109.5 . . ? C78 C783 H78G 109.5 . . ? C78 C783 H78H 109.5 . . ? H78G C783 H78H 109.5 . . ? C78 C783 H78I 109.5 . . ? H78G C783 H78I 109.5 . . ? H78H C783 H78I 109.5 . . ? C86 C81 C82 120.1(5) . . ? C86 C81 H81A 119.9 . . ? C82 C81 H81A 119.9 . . ? C83 C82 C81 120.0(5) . . ? C83 C82 H82A 120.0 . . ? C81 C82 H82A 120.0 . . ? C82 C83 C84 119.4(5) . . ? C82 C83 H83A 120.3 . . ? C84 C83 H83A 120.3 . . ? C85 C84 C83 120.5(5) . . ? C85 C84 H84A 119.8 . . ? C83 C84 H84A 119.8 . . ? C86 C85 C84 119.8(5) . . ? C86 C85 H85A 120.1 . . ? C84 C85 H85A 120.1 . . ? C85 C86 C81 120.1(5) . . ? C85 C86 H86A 119.9 . . ? C81 C86 H86A 119.9 . . ? C92 C91 C93 119.9(5) . 2_745 ? C92 C91 H91A 120.0 . . ? C93 C91 H91A 120.0 2_745 . ? C93 C92 C91 120.1(5) . . ? C93 C92 H92A 120.0 . . ? C91 C92 H92A 120.0 . . ? C92 C93 C91 120.0(5) . 2_745 ? C92 C93 H93A 120.0 . . ? C91 C93 H93A 120.0 2_745 . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.139 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.099 _database_code_depnum_ccdc_archive 'CCDC 976191' ####################################################################### # # 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_ss1140m _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis(3,5-di-tert-butylcatecholato)dioxodimolybedenum(VI) di-benzene solvate ; _chemical_name_common '(3,5tBuCat)4Mo2O2 . 2 C6H6' _chemical_melting_point ? _chemical_formula_moiety 'C56 H80 Mo2 O10, 2(C6 H6)' _chemical_formula_sum 'C68 H92 Mo2 O10' _chemical_formula_weight 1261.30 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 11.7617(3) _cell_length_b 16.6561(4) _cell_length_c 16.5304(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.3779(11) _cell_angle_gamma 90.00 _cell_volume 3238.30(14) _cell_formula_units_Z 2 _cell_measurement_temperature 119(2) _cell_measurement_reflns_used 9804 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.86 _exptl_crystal_description tablet _exptl_crystal_colour brown _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.442 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7990 _exptl_absorpt_correction_T_max 0.9302 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G. M. (2004) SADABS, University of Gottingen, Germany. ; _exptl_crystal_recrystallization_method ; Crystals were grown from C6H6/CH3CN in a recrystallization attempt of (tBuClip)Mo(\m-3,5-tBu2Cat)2Mo(O)(3,5-tBu2Cat) that was exposed to air. ; _exptl_special_details ; ; _diffrn_ambient_temperature 119(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 Apex II CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 37715 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0156 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.30 _reflns_number_total 7332 _reflns_number_gt 6694 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. All hydrogens on non disordered carbons were found in difference Fourier maps and were refined isotropically. The 3 methyl groups on C18 were refined in two different orientations; the occupancy of the minor orientation refined to 0.121(7). ; _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^)+(0.0275P)^2^+2.0577P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7332 _refine_ls_number_parameters 519 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0561 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.507278(9) 0.951144(6) 0.594047(6) 0.01179(4) Uani 1 1 d . . . O1 O 0.63923(8) 0.89524(6) 0.55241(6) 0.01591(19) Uani 1 1 d . . . O2 O 0.62705(8) 0.98896(6) 0.66649(5) 0.01520(19) Uani 1 1 d . . . O4 O 0.42370(8) 1.03989(5) 0.63845(6) 0.01430(18) Uani 1 1 d . . . O O 0.43310(8) 0.87785(6) 0.64000(6) 0.0182(2) Uani 1 1 d . . . C11 C 0.74277(11) 0.91482(8) 0.58359(8) 0.0159(3) Uani 1 1 d . . . C12 C 0.73613(11) 0.96899(8) 0.64794(8) 0.0153(3) Uani 1 1 d . . . C13 C 0.83385(12) 0.99614(8) 0.68834(8) 0.0175(3) Uani 1 1 d . . . C14 C 0.93613(12) 0.96329(9) 0.66104(9) 0.0196(3) Uani 1 1 d . . . H14 H 1.0040(15) 0.9813(10) 0.6866(10) 0.019(4) Uiso 1 1 d . . . C15 C 0.94439(12) 0.90729(8) 0.59762(9) 0.0189(3) Uani 1 1 d . A . C16 C 0.84514(12) 0.88273(9) 0.55820(9) 0.0190(3) Uani 1 1 d . . . H16 H 0.8438(14) 0.8456(10) 0.5162(10) 0.019(4) Uiso 1 1 d . . . C17 C 0.82739(13) 1.05847(9) 0.75638(9) 0.0220(3) Uani 1 1 d . . . C18 C 1.06077(12) 0.87259(9) 0.57442(10) 0.0229(3) Uani 1 1 d . . . C21 C 0.53628(11) 1.12916(8) 0.56605(8) 0.0140(2) Uani 1 1 d . . . C22 C 0.46439(11) 1.11542(8) 0.63219(8) 0.0138(2) Uani 1 1 d . . . C23 C 0.43870(11) 1.17786(8) 0.68674(8) 0.0152(3) Uani 1 1 d . . . C24 C 0.48805(11) 1.25184(8) 0.67005(8) 0.0169(3) Uani 1 1 d . . . H24 H 0.4750(13) 1.2961(10) 0.7058(10) 0.016(4) Uiso 1 1 d . . . C25 C 0.55846(12) 1.26679(8) 0.60293(8) 0.0165(3) Uani 1 1 d . . . C26 C 0.58128(12) 1.20392(8) 0.54976(8) 0.0161(3) Uani 1 1 d . . . H26 H 0.6268(14) 1.2111(10) 0.5056(10) 0.020(4) Uiso 1 1 d . . . C27 C 0.36501(12) 1.16324(8) 0.76167(8) 0.0192(3) Uani 1 1 d . . . C28 C 0.60677(13) 1.35131(8) 0.59091(8) 0.0203(3) Uani 1 1 d . . . C81 C 0.1094(2) 1.38440(17) 0.48946(15) 0.0581(6) Uani 1 1 d . . . C82 C 0.0137(2) 1.39611(15) 0.53541(18) 0.0584(7) Uani 1 1 d . . . C83 C 0.00717(17) 1.36416(14) 0.61166(16) 0.0509(5) Uani 1 1 d . . . C84 C 0.09688(19) 1.31980(14) 0.64281(14) 0.0479(5) Uani 1 1 d . . . C85 C 0.19234(17) 1.30780(13) 0.59602(13) 0.0412(4) Uani 1 1 d . . . C86 C 0.19873(18) 1.34026(14) 0.51963(12) 0.0457(5) Uani 1 1 d . . . C171 C 0.94559(15) 1.07977(12) 0.78941(12) 0.0333(4) Uani 1 1 d . . . H17C H 0.9834(17) 1.0330(12) 0.8108(12) 0.032(5) Uiso 1 1 d . . . H17B H 0.9930(18) 1.1034(13) 0.7472(13) 0.042(6) Uiso 1 1 d . . . H17A H 0.9359(18) 1.1187(13) 0.8327(13) 0.042(6) Uiso 1 1 d . . . C172 C 0.75573(16) 1.02514(12) 0.82600(10) 0.0305(4) Uani 1 1 d . . . H17F H 0.7879(17) 0.9766(13) 0.8487(12) 0.036(5) Uiso 1 1 d . . . H17E H 0.6826(18) 1.0129(12) 0.8098(12) 0.035(5) Uiso 1 1 d . . . H17D H 0.7517(18) 1.0654(13) 0.8692(13) 0.042(6) Uiso 1 1 d . . . C173 C 0.77278(15) 1.13626(10) 0.72380(11) 0.0274(3) Uani 1 1 d . . . H17I H 0.8168(17) 1.1584(12) 0.6806(12) 0.035(5) Uiso 1 1 d . . . H17H H 0.6975(16) 1.1273(11) 0.7040(11) 0.028(5) Uiso 1 1 d . . . H17G H 0.7671(17) 1.1754(12) 0.7670(12) 0.036(5) Uiso 1 1 d . . . C184 C 1.069(3) 0.866(3) 0.496(2) 0.0673(13) Uani 0.121(7) 1 d P A 1 H18A H 1.0957 0.9175 0.4738 0.101 Uiso 0.121(7) 1 calc PR A 1 H18B H 0.9941 0.8536 0.4730 0.101 Uiso 0.121(7) 1 calc PR A 1 H18C H 1.1228 0.8237 0.4828 0.101 Uiso 0.121(7) 1 calc PR A 1 C185 C 1.156(2) 0.9139(17) 0.6175(16) 0.0812(17) Uani 0.121(7) 1 d P A 1 H18D H 1.1315 0.9290 0.6720 0.122 Uiso 0.121(7) 1 calc PR A 1 H18E H 1.1775 0.9623 0.5875 0.122 Uiso 0.121(7) 1 calc PR A 1 H18F H 1.2214 0.8777 0.6214 0.122 Uiso 0.121(7) 1 calc PR A 1 C186 C 1.063(2) 0.7914(17) 0.628(3) 0.0633(14) Uani 0.121(7) 1 d P A 1 H18G H 1.0685 0.8055 0.6856 0.095 Uiso 0.121(7) 1 calc PR A 1 H18H H 1.1293 0.7590 0.6130 0.095 Uiso 0.121(7) 1 calc PR A 1 H18I H 0.9935 0.7607 0.6182 0.095 Uiso 0.121(7) 1 calc PR A 1 C181 C 1.0605(3) 0.8396(3) 0.4870(3) 0.0673(13) Uani 0.879(7) 1 d P A 2 H18J H 1.0296 0.8803 0.4502 0.101 Uiso 0.879(7) 1 calc PR A 2 H18K H 1.0132 0.7912 0.4843 0.101 Uiso 0.879(7) 1 calc PR A 2 H18L H 1.1384 0.8264 0.4712 0.101 Uiso 0.879(7) 1 calc PR A 2 C182 C 1.0922(4) 0.8062(3) 0.6313(3) 0.0812(17) Uani 0.879(7) 1 d P A 2 H18M H 1.0972 0.8274 0.6866 0.122 Uiso 0.879(7) 1 calc PR A 2 H18N H 1.1658 0.7837 0.6158 0.122 Uiso 0.879(7) 1 calc PR A 2 H18O H 1.0340 0.7641 0.6289 0.122 Uiso 0.879(7) 1 calc PR A 2 C183 C 1.1522(2) 0.93736(17) 0.5751(3) 0.0633(14) Uani 0.879(7) 1 d P A 2 H18P H 1.1547 0.9631 0.6284 0.095 Uiso 0.879(7) 1 calc PR A 2 H18Q H 1.1345 0.9777 0.5337 0.095 Uiso 0.879(7) 1 calc PR A 2 H18R H 1.2262 0.9130 0.5637 0.095 Uiso 0.879(7) 1 calc PR A 2 C271 C 0.34068(15) 1.24142(10) 0.80728(10) 0.0267(3) Uani 1 1 d . . . H27C H 0.3041(15) 1.2811(11) 0.7730(11) 0.026(5) Uiso 1 1 d . . . H27B H 0.4073(17) 1.2629(12) 0.8284(11) 0.030(5) Uiso 1 1 d . . . C272 C 0.25037(14) 1.12505(11) 0.73791(11) 0.0276(3) Uani 1 1 d . . . H27F H 0.2110(16) 1.1572(12) 0.7004(12) 0.030(5) Uiso 1 1 d . . . H27D H 0.2580(17) 1.0721(13) 0.7132(13) 0.039(5) Uiso 1 1 d . . . C273 C 0.42953(16) 1.10604(11) 0.81850(10) 0.0283(3) Uani 1 1 d . . . H27I H 0.5030(18) 1.1300(13) 0.8343(12) 0.040(6) Uiso 1 1 d . . . H27H H 0.4471(17) 1.0554(12) 0.7919(12) 0.033(5) Uiso 1 1 d . . . H27G H 0.3838(16) 1.0966(12) 0.8665(12) 0.032(5) Uiso 1 1 d . . . C281 C 0.50770(17) 1.41044(10) 0.58078(13) 0.0361(4) Uani 1 1 d . . . H28C H 0.463(2) 1.3964(14) 0.5341(14) 0.053(7) Uiso 1 1 d . . . H28B H 0.4576(19) 1.4115(14) 0.6301(14) 0.049(6) Uiso 1 1 d . . . H28A H 0.5394(19) 1.4630(13) 0.5736(13) 0.043(6) Uiso 1 1 d . . . C282 C 0.68238(18) 1.35659(11) 0.51636(11) 0.0341(4) Uani 1 1 d . . . H28F H 0.7498(18) 1.3207(13) 0.5207(12) 0.037(5) Uiso 1 1 d . . . H28E H 0.6427(19) 1.3432(13) 0.4700(14) 0.046(6) Uiso 1 1 d . . . H28D H 0.7103(17) 1.4097(13) 0.5112(12) 0.039(5) Uiso 1 1 d . . . C283 C 0.67854(15) 1.37430(11) 0.66529(10) 0.0275(3) Uani 1 1 d . . . H28I H 0.7384(18) 1.3367(13) 0.6710(12) 0.039(6) Uiso 1 1 d . . . H28H H 0.7132(18) 1.4258(13) 0.6564(12) 0.039(5) Uiso 1 1 d . . . H28G H 0.6329(16) 1.3764(11) 0.7123(12) 0.030(5) Uiso 1 1 d . . . H27E H 0.2049(18) 1.1199(13) 0.7855(13) 0.043(6) Uiso 1 1 d . . . H85 H 0.255(2) 1.2776(15) 0.6156(14) 0.059(7) Uiso 1 1 d . . . H86 H 0.268(2) 1.3298(15) 0.4895(15) 0.059(7) Uiso 1 1 d . . . H83 H -0.057(2) 1.3704(15) 0.6471(15) 0.065(8) Uiso 1 1 d . . . H84 H 0.090(2) 1.2959(16) 0.6987(16) 0.067(8) Uiso 1 1 d . . . H81 H 0.125(2) 1.4099(19) 0.4379(18) 0.087(9) Uiso 1 1 d . . . H82 H -0.050(3) 1.427(2) 0.5138(19) 0.096(10) Uiso 1 1 d . . . H27A H 0.2899(17) 1.2311(12) 0.8509(12) 0.034(5) Uiso 1 1 d . . . O3 O 0.55754(8) 1.06233(5) 0.51962(5) 0.01382(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 Mo1 0.01208(6) 0.01146(6) 0.01183(6) -0.00049(4) 0.00084(4) -0.00032(4) O1 0.0140(4) 0.0164(5) 0.0172(5) -0.0034(4) -0.0009(4) 0.0008(4) O2 0.0136(4) 0.0173(5) 0.0147(4) -0.0019(4) -0.0005(3) 0.0003(4) O4 0.0135(4) 0.0132(4) 0.0162(4) -0.0013(3) 0.0015(3) -0.0008(3) O 0.0202(5) 0.0162(5) 0.0182(5) 0.0009(4) 0.0026(4) -0.0015(4) C11 0.0153(6) 0.0150(6) 0.0173(6) 0.0010(5) -0.0011(5) -0.0009(5) C12 0.0148(6) 0.0162(6) 0.0150(6) 0.0013(5) 0.0014(5) 0.0016(5) C13 0.0182(7) 0.0183(7) 0.0159(6) 0.0009(5) -0.0013(5) -0.0004(5) C14 0.0159(7) 0.0217(7) 0.0212(7) 0.0012(5) -0.0029(5) -0.0010(5) C15 0.0157(6) 0.0177(7) 0.0232(7) 0.0033(5) 0.0019(5) 0.0019(5) C16 0.0196(7) 0.0169(7) 0.0204(7) -0.0020(5) 0.0019(5) 0.0017(5) C17 0.0191(7) 0.0265(8) 0.0204(7) -0.0067(6) -0.0038(6) 0.0000(6) C18 0.0153(7) 0.0225(7) 0.0308(8) 0.0010(6) 0.0019(6) 0.0044(6) C21 0.0134(6) 0.0147(6) 0.0138(6) -0.0026(5) -0.0022(5) 0.0007(5) C22 0.0127(6) 0.0128(6) 0.0160(6) 0.0005(5) -0.0005(5) -0.0003(5) C23 0.0142(6) 0.0164(6) 0.0150(6) -0.0012(5) 0.0007(5) 0.0010(5) C24 0.0189(7) 0.0150(7) 0.0168(6) -0.0028(5) 0.0013(5) 0.0005(5) C25 0.0178(6) 0.0149(6) 0.0167(6) -0.0004(5) -0.0014(5) -0.0016(5) C26 0.0166(6) 0.0178(7) 0.0138(6) 0.0002(5) 0.0009(5) -0.0013(5) C27 0.0208(7) 0.0177(7) 0.0193(7) -0.0027(5) 0.0062(5) -0.0014(5) C28 0.0275(7) 0.0149(7) 0.0186(7) -0.0016(5) 0.0031(6) -0.0048(6) C81 0.0582(15) 0.0720(17) 0.0439(12) 0.0111(11) -0.0189(11) -0.0132(12) C82 0.0429(12) 0.0447(12) 0.0874(19) 0.0064(12) -0.0278(13) 0.0002(10) C83 0.0301(10) 0.0455(12) 0.0772(16) -0.0111(11) 0.0064(10) -0.0020(9) C84 0.0417(11) 0.0526(13) 0.0496(12) 0.0073(10) 0.0059(9) -0.0022(9) C85 0.0325(10) 0.0446(11) 0.0465(11) 0.0002(9) -0.0054(8) 0.0050(8) C86 0.0387(11) 0.0615(14) 0.0368(10) -0.0129(9) -0.0011(8) -0.0069(10) C171 0.0251(8) 0.0384(10) 0.0361(9) -0.0156(8) -0.0109(7) 0.0011(7) C172 0.0315(9) 0.0423(10) 0.0177(7) -0.0044(7) 0.0003(6) 0.0032(8) C173 0.0278(8) 0.0233(8) 0.0309(8) -0.0077(7) -0.0063(7) 0.0006(6) C184 0.0281(13) 0.125(4) 0.0491(17) -0.043(2) 0.0005(11) 0.031(2) C185 0.065(3) 0.087(3) 0.092(2) 0.068(2) 0.048(2) 0.060(2) C186 0.0194(10) 0.0360(14) 0.135(4) -0.0206(17) 0.0290(15) -0.0057(9) C181 0.0281(13) 0.125(4) 0.0491(17) -0.043(2) 0.0005(11) 0.031(2) C182 0.065(3) 0.087(3) 0.092(2) 0.068(2) 0.048(2) 0.060(2) C183 0.0194(10) 0.0360(14) 0.135(4) -0.0206(17) 0.0290(15) -0.0057(9) C271 0.0329(9) 0.0218(8) 0.0256(8) -0.0069(6) 0.0133(7) -0.0036(7) C272 0.0210(7) 0.0285(8) 0.0334(9) -0.0070(7) 0.0095(7) -0.0048(6) C273 0.0374(9) 0.0284(8) 0.0192(7) 0.0028(6) 0.0064(7) 0.0027(7) C281 0.0409(10) 0.0159(8) 0.0515(11) 0.0044(7) -0.0045(9) -0.0003(7) C282 0.0551(12) 0.0228(8) 0.0245(8) -0.0038(7) 0.0146(8) -0.0178(8) C283 0.0337(9) 0.0261(8) 0.0226(8) -0.0022(6) 0.0012(7) -0.0126(7) O3 0.0144(4) 0.0131(4) 0.0139(4) -0.0024(3) 0.0002(3) -0.0002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O 1.6844(10) . ? Mo1 O4 1.9233(9) . ? Mo1 O1 1.9400(9) . ? Mo1 O2 1.9476(9) . ? Mo1 O3 2.0354(9) 3_676 ? Mo1 O3 2.3027(9) . ? O1 C11 1.3590(16) . ? O2 C12 1.3623(16) . ? O4 C22 1.3503(16) . ? C11 C16 1.3849(19) . ? C11 C12 1.3975(19) . ? C12 C13 1.4003(19) . ? C13 C14 1.399(2) . ? C13 C17 1.5329(19) . ? C14 C15 1.407(2) . ? C14 H14 0.949(18) . ? C15 C16 1.395(2) . ? C15 C18 1.5368(19) . ? C16 H16 0.929(17) . ? C17 C171 1.532(2) . ? C17 C172 1.535(2) . ? C17 C173 1.542(2) . ? C18 C184 1.30(4) . ? C18 C185 1.49(3) . ? C18 C182 1.496(3) . ? C18 C183 1.523(3) . ? C18 C181 1.546(4) . ? C18 C186 1.62(3) . ? C21 O3 1.3759(15) . ? C21 C26 1.3803(19) . ? C21 C22 1.4053(18) . ? C22 C23 1.4105(18) . ? C23 C24 1.3907(19) . ? C23 C27 1.5358(18) . ? C24 C25 1.4110(19) . ? C24 H24 0.957(17) . ? C25 C26 1.3943(19) . ? C25 C28 1.5315(19) . ? C26 H26 0.915(17) . ? C27 C271 1.533(2) . ? C27 C273 1.535(2) . ? C27 C272 1.539(2) . ? C28 C282 1.527(2) . ? C28 C281 1.534(2) . ? C28 C283 1.535(2) . ? C81 C86 1.373(3) . ? C81 C82 1.376(4) . ? C81 H81 0.97(3) . ? C82 C83 1.371(4) . ? C82 H82 0.97(3) . ? C83 C84 1.385(3) . ? C83 H83 0.96(3) . ? C84 C85 1.382(3) . ? C84 H84 1.01(3) . ? C85 C86 1.376(3) . ? C85 H85 0.94(2) . ? C86 H86 0.98(2) . ? C171 H17C 0.96(2) . ? C171 H17B 0.98(2) . ? C171 H17A 0.97(2) . ? C172 H17F 0.97(2) . ? C172 H17E 0.92(2) . ? C172 H17D 0.98(2) . ? C173 H17I 0.96(2) . ? C173 H17H 0.954(19) . ? C173 H17G 0.97(2) . ? C184 H18A 0.9800 . ? C184 H18B 0.9800 . ? C184 H18C 0.9800 . ? C185 H18D 0.9800 . ? C185 H18E 0.9800 . ? C185 H18F 0.9800 . ? C186 H18G 0.9800 . ? C186 H18H 0.9800 . ? C186 H18I 0.9800 . ? C181 H18J 0.9800 . ? C181 H18K 0.9800 . ? C181 H18L 0.9800 . ? C182 H18M 0.9800 . ? C182 H18N 0.9800 . ? C182 H18O 0.9800 . ? C183 H18P 0.9800 . ? C183 H18Q 0.9800 . ? C183 H18R 0.9800 . ? C271 H27C 0.969(19) . ? C271 H27B 0.93(2) . ? C271 H27A 0.95(2) . ? C272 H27F 0.94(2) . ? C272 H27D 0.98(2) . ? C272 H27E 0.96(2) . ? C273 H27I 0.99(2) . ? C273 H27H 0.97(2) . ? C273 H27G 0.97(2) . ? C281 H28C 0.96(2) . ? C281 H28B 1.01(2) . ? C281 H28A 0.96(2) . ? C282 H28F 0.99(2) . ? C282 H28E 0.92(2) . ? C282 H28D 0.95(2) . ? C283 H28I 0.95(2) . ? C283 H28H 0.96(2) . ? C283 H28G 0.95(2) . ? O3 Mo1 2.0355(9) 3_676 ? 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 O Mo1 O4 96.74(4) . . ? O Mo1 O1 103.31(4) . . ? O4 Mo1 O1 156.39(4) . . ? O Mo1 O2 109.38(4) . . ? O4 Mo1 O2 83.47(4) . . ? O1 Mo1 O2 78.24(4) . . ? O Mo1 O3 98.30(4) . 3_676 ? O4 Mo1 O3 104.34(4) . 3_676 ? O1 Mo1 O3 85.14(4) . 3_676 ? O2 Mo1 O3 150.26(4) . 3_676 ? O Mo1 O3 163.61(4) . . ? O4 Mo1 O3 73.71(4) . . ? O1 Mo1 O3 89.29(4) . . ? O2 Mo1 O3 83.18(4) . . ? O3 Mo1 O3 72.02(4) 3_676 . ? C11 O1 Mo1 117.86(8) . . ? C12 O2 Mo1 117.46(8) . . ? C22 O4 Mo1 120.30(8) . . ? O1 C11 C16 124.83(12) . . ? O1 C11 C12 112.90(12) . . ? C16 C11 C12 122.20(13) . . ? O2 C12 C11 112.73(12) . . ? O2 C12 C13 125.81(12) . . ? C11 C12 C13 121.44(12) . . ? C14 C13 C12 115.13(13) . . ? C14 C13 C17 123.25(13) . . ? C12 C13 C17 121.61(12) . . ? C13 C14 C15 124.28(13) . . ? C13 C14 H14 117.1(10) . . ? C15 C14 H14 118.6(10) . . ? C16 C15 C14 118.75(13) . . ? C16 C15 C18 121.15(13) . . ? C14 C15 C18 120.08(13) . . ? C11 C16 C15 118.16(13) . . ? C11 C16 H16 118.2(10) . . ? C15 C16 H16 123.7(10) . . ? C171 C17 C13 111.66(13) . . ? C171 C17 C172 108.55(14) . . ? C13 C17 C172 109.59(13) . . ? C171 C17 C173 107.76(14) . . ? C13 C17 C173 109.59(12) . . ? C172 C17 C173 109.65(14) . . ? C184 C18 C185 117(2) . . ? C182 C18 C183 110.3(2) . . ? C184 C18 C15 110.4(16) . . ? C185 C18 C15 112.0(8) . . ? C182 C18 C15 109.72(16) . . ? C183 C18 C15 111.20(14) . . ? C182 C18 C181 108.9(3) . . ? C183 C18 C181 104.8(3) . . ? C15 C18 C181 111.74(18) . . ? C184 C18 C186 119(3) . . ? C185 C18 C186 96.5(14) . . ? C15 C18 C186 101.0(10) . . ? O3 C21 C26 123.35(12) . . ? O3 C21 C22 114.50(11) . . ? C26 C21 C22 122.14(12) . . ? O4 C22 C21 115.26(11) . . ? O4 C22 C23 124.08(12) . . ? C21 C22 C23 120.66(12) . . ? C24 C23 C22 115.78(12) . . ? C24 C23 C27 122.62(12) . . ? C22 C23 C27 121.55(12) . . ? C23 C24 C25 124.08(13) . . ? C23 C24 H24 119.4(10) . . ? C25 C24 H24 116.5(10) . . ? C26 C25 C24 118.65(12) . . ? C26 C25 C28 122.38(12) . . ? C24 C25 C28 118.97(12) . . ? C21 C26 C25 118.62(12) . . ? C21 C26 H26 120.0(11) . . ? C25 C26 H26 121.3(11) . . ? C271 C27 C273 108.63(13) . . ? C271 C27 C23 111.73(12) . . ? C273 C27 C23 108.21(12) . . ? C271 C27 C272 108.09(13) . . ? C273 C27 C272 109.16(13) . . ? C23 C27 C272 110.96(12) . . ? C282 C28 C25 112.09(12) . . ? C282 C28 C281 108.72(15) . . ? C25 C28 C281 108.79(13) . . ? C282 C28 C283 108.17(14) . . ? C25 C28 C283 109.14(12) . . ? C281 C28 C283 109.92(14) . . ? C86 C81 C82 120.1(2) . . ? C86 C81 H81 114.1(18) . . ? C82 C81 H81 125.4(18) . . ? C83 C82 C81 120.2(2) . . ? C83 C82 H82 119.7(19) . . ? C81 C82 H82 120.1(19) . . ? C82 C83 C84 120.1(2) . . ? C82 C83 H83 124.5(16) . . ? C84 C83 H83 115.4(16) . . ? C85 C84 C83 119.3(2) . . ? C85 C84 H84 121.6(15) . . ? C83 C84 H84 119.1(15) . . ? C86 C85 C84 120.4(2) . . ? C86 C85 H85 118.4(15) . . ? C84 C85 H85 121.2(15) . . ? C81 C86 C85 119.8(2) . . ? C81 C86 H86 123.5(15) . . ? C85 C86 H86 116.7(15) . . ? C17 C171 H17C 111.1(12) . . ? C17 C171 H17B 111.1(13) . . ? H17C C171 H17B 108.8(17) . . ? C17 C171 H17A 107.8(12) . . ? H17C C171 H17A 109.0(17) . . ? H17B C171 H17A 109.0(17) . . ? C17 C172 H17F 112.2(12) . . ? C17 C172 H17E 112.3(12) . . ? H17F C172 H17E 106.8(17) . . ? C17 C172 H17D 109.1(13) . . ? H17F C172 H17D 108.0(17) . . ? H17E C172 H17D 108.3(17) . . ? C17 C173 H17I 111.0(12) . . ? C17 C173 H17H 111.9(11) . . ? H17I C173 H17H 108.0(16) . . ? C17 C173 H17G 109.8(12) . . ? H17I C173 H17G 109.3(16) . . ? H17H C173 H17G 106.8(16) . . ? C18 C184 H18A 109.5 . . ? C18 C184 H18B 109.5 . . ? H18A C184 H18B 109.5 . . ? C18 C184 H18C 109.5 . . ? H18A C184 H18C 109.5 . . ? H18B C184 H18C 109.5 . . ? C18 C185 H18D 109.5 . . ? C18 C185 H18E 109.5 . . ? H18D C185 H18E 109.5 . . ? C18 C185 H18F 109.5 . . ? H18D C185 H18F 109.5 . . ? H18E C185 H18F 109.5 . . ? C18 C186 H18G 109.5 . . ? C18 C186 H18H 109.5 . . ? H18G C186 H18H 109.5 . . ? C18 C186 H18I 109.5 . . ? H18G C186 H18I 109.5 . . ? H18H C186 H18I 109.5 . . ? C18 C181 H18J 109.5 . . ? C18 C181 H18K 109.5 . . ? H18J C181 H18K 109.5 . . ? C18 C181 H18L 109.5 . . ? H18J C181 H18L 109.5 . . ? H18K C181 H18L 109.5 . . ? C18 C182 H18M 109.5 . . ? C18 C182 H18N 109.5 . . ? H18M C182 H18N 109.5 . . ? C18 C182 H18O 109.5 . . ? H18M C182 H18O 109.5 . . ? H18N C182 H18O 109.5 . . ? C18 C183 H18P 109.5 . . ? C18 C183 H18Q 109.5 . . ? H18P C183 H18Q 109.5 . . ? C18 C183 H18R 109.5 . . ? H18P C183 H18R 109.5 . . ? H18Q C183 H18R 109.5 . . ? C27 C271 H27C 112.1(11) . . ? C27 C271 H27B 110.7(12) . . ? H27C C271 H27B 109.1(16) . . ? C27 C271 H27A 109.7(12) . . ? H27C C271 H27A 106.6(16) . . ? H27B C271 H27A 108.4(16) . . ? C27 C272 H27F 111.1(12) . . ? C27 C272 H27D 113.4(12) . . ? H27F C272 H27D 106.6(16) . . ? C27 C272 H27E 108.7(13) . . ? H27F C272 H27E 108.5(17) . . ? H27D C272 H27E 108.4(17) . . ? C27 C273 H27I 109.9(12) . . ? C27 C273 H27H 111.5(12) . . ? H27I C273 H27H 106.3(17) . . ? C27 C273 H27G 109.0(11) . . ? H27I C273 H27G 109.7(16) . . ? H27H C273 H27G 110.4(16) . . ? C28 C281 H28C 110.2(14) . . ? C28 C281 H28B 111.7(13) . . ? H28C C281 H28B 109.4(19) . . ? C28 C281 H28A 107.7(13) . . ? H28C C281 H28A 109.5(19) . . ? H28B C281 H28A 108.2(18) . . ? C28 C282 H28F 112.0(12) . . ? C28 C282 H28E 111.3(14) . . ? H28F C282 H28E 108.3(18) . . ? C28 C282 H28D 109.3(12) . . ? H28F C282 H28D 106.9(17) . . ? H28E C282 H28D 109.0(18) . . ? C28 C283 H28I 108.7(13) . . ? C28 C283 H28H 109.4(12) . . ? H28I C283 H28H 106.8(17) . . ? C28 C283 H28G 110.8(11) . . ? H28I C283 H28G 111.5(17) . . ? H28H C283 H28G 109.6(17) . . ? C21 O3 Mo1 122.39(8) . 3_676 ? C21 O3 Mo1 107.72(7) . . ? Mo1 O3 Mo1 107.98(4) 3_676 . ? 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 O Mo1 O1 C11 -114.80(9) . . . . ? O4 Mo1 O1 C11 32.57(15) . . . . ? O2 Mo1 O1 C11 -7.40(9) . . . . ? O3 Mo1 O1 C11 147.80(9) 3_676 . . . ? O3 Mo1 O1 C11 75.78(9) . . . . ? O Mo1 O2 C12 108.31(9) . . . . ? O4 Mo1 O2 C12 -156.82(9) . . . . ? O1 Mo1 O2 C12 8.17(9) . . . . ? O3 Mo1 O2 C12 -49.23(13) 3_676 . . . ? O3 Mo1 O2 C12 -82.53(9) . . . . ? O Mo1 O4 C22 167.02(9) . . . . ? O1 Mo1 O4 C22 18.91(16) . . . . ? O2 Mo1 O4 C22 58.19(9) . . . . ? O3 Mo1 O4 C22 -92.59(9) 3_676 . . . ? O3 Mo1 O4 C22 -26.58(9) . . . . ? Mo1 O1 C11 C16 -177.40(11) . . . . ? Mo1 O1 C11 C12 5.49(15) . . . . ? Mo1 O2 C12 C11 -7.61(14) . . . . ? Mo1 O2 C12 C13 174.13(11) . . . . ? O1 C11 C12 O2 1.35(16) . . . . ? C16 C11 C12 O2 -175.85(12) . . . . ? O1 C11 C12 C13 179.70(12) . . . . ? C16 C11 C12 C13 2.5(2) . . . . ? O2 C12 C13 C14 176.29(13) . . . . ? C11 C12 C13 C14 -1.8(2) . . . . ? O2 C12 C13 C17 -4.7(2) . . . . ? C11 C12 C13 C17 177.16(13) . . . . ? C12 C13 C14 C15 0.3(2) . . . . ? C17 C13 C14 C15 -178.63(14) . . . . ? C13 C14 C15 C16 0.6(2) . . . . ? C13 C14 C15 C18 -177.76(13) . . . . ? O1 C11 C16 C15 -178.34(13) . . . . ? C12 C11 C16 C15 -1.5(2) . . . . ? C14 C15 C16 C11 0.0(2) . . . . ? C18 C15 C16 C11 178.30(13) . . . . ? C14 C13 C17 C171 0.3(2) . . . . ? C12 C13 C17 C171 -178.61(14) . . . . ? C14 C13 C17 C172 -120.02(15) . . . . ? C12 C13 C17 C172 61.07(18) . . . . ? C14 C13 C17 C173 119.61(15) . . . . ? C12 C13 C17 C173 -59.29(18) . . . . ? C16 C15 C18 C184 41(2) . . . . ? C14 C15 C18 C184 -140(2) . . . . ? C16 C15 C18 C185 173.5(9) . . . . ? C14 C15 C18 C185 -8.2(9) . . . . ? C16 C15 C18 C182 -97.5(3) . . . . ? C14 C15 C18 C182 80.8(3) . . . . ? C16 C15 C18 C183 140.2(2) . . . . ? C14 C15 C18 C183 -41.5(3) . . . . ? C16 C15 C18 C181 23.4(3) . . . . ? C14 C15 C18 C181 -158.3(3) . . . . ? C16 C15 C18 C186 -84.8(13) . . . . ? C14 C15 C18 C186 93.4(13) . . . . ? Mo1 O4 C22 C21 26.53(15) . . . . ? Mo1 O4 C22 C23 -153.51(10) . . . . ? O3 C21 C22 O4 -2.42(17) . . . . ? C26 C21 C22 O4 177.60(12) . . . . ? O3 C21 C22 C23 177.61(11) . . . . ? C26 C21 C22 C23 -2.4(2) . . . . ? O4 C22 C23 C24 -179.57(12) . . . . ? C21 C22 C23 C24 0.39(19) . . . . ? O4 C22 C23 C27 3.0(2) . . . . ? C21 C22 C23 C27 -177.04(12) . . . . ? C22 C23 C24 C25 1.0(2) . . . . ? C27 C23 C24 C25 178.35(13) . . . . ? C23 C24 C25 C26 -0.4(2) . . . . ? C23 C24 C25 C28 179.45(13) . . . . ? O3 C21 C26 C25 -177.06(12) . . . . ? C22 C21 C26 C25 2.9(2) . . . . ? C24 C25 C26 C21 -1.5(2) . . . . ? C28 C25 C26 C21 178.63(12) . . . . ? C24 C23 C27 C271 7.70(19) . . . . ? C22 C23 C27 C271 -175.05(13) . . . . ? C24 C23 C27 C273 -111.84(15) . . . . ? C22 C23 C27 C273 65.40(17) . . . . ? C24 C23 C27 C272 128.41(15) . . . . ? C22 C23 C27 C272 -54.34(18) . . . . ? C26 C25 C28 C282 -1.1(2) . . . . ? C24 C25 C28 C282 179.10(14) . . . . ? C26 C25 C28 C281 119.20(16) . . . . ? C24 C25 C28 C281 -60.63(17) . . . . ? C26 C25 C28 C283 -120.87(15) . . . . ? C24 C25 C28 C283 59.30(17) . . . . ? C86 C81 C82 C83 0.3(4) . . . . ? C81 C82 C83 C84 -0.1(4) . . . . ? C82 C83 C84 C85 -0.4(4) . . . . ? C83 C84 C85 C86 0.7(3) . . . . ? C82 C81 C86 C85 -0.1(4) . . . . ? C84 C85 C86 C81 -0.4(3) . . . . ? C26 C21 O3 Mo1 -70.68(15) . . . 3_676 ? C22 C21 O3 Mo1 109.34(11) . . . 3_676 ? C26 C21 O3 Mo1 163.41(11) . . . . ? C22 C21 O3 Mo1 -16.57(13) . . . . ? O Mo1 O3 C21 78.44(16) . . . . ? O4 Mo1 O3 C21 22.55(8) . . . . ? O1 Mo1 O3 C21 -140.86(8) . . . . ? O2 Mo1 O3 C21 -62.61(8) . . . . ? O3 Mo1 O3 C21 134.03(9) 3_676 . . . ? O Mo1 O3 Mo1 -55.58(15) . . . 3_676 ? O4 Mo1 O3 Mo1 -111.48(5) . . . 3_676 ? O1 Mo1 O3 Mo1 85.12(4) . . . 3_676 ? O2 Mo1 O3 Mo1 163.36(5) . . . 3_676 ? O3 Mo1 O3 Mo1 0.0 3_676 . . 3_676 ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.567 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.050 _vrf_PLAT220_ss1140m ; RESPONSE: Large C and H thermal displacement parameters reported here are due to the disordered tBu groups. Thermal parameters on tBu groups were refined anisotropically. This also leads to the B alert for hydrogen atoms below. See _refine_special_details for the analysis of the disorder. ; _database_code_depnum_ccdc_archive 'CCDC 976192'