# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_cy477 _database_code_depnum_ccdc_archive 'CCDC 909163' #TrackingRef 'MnMo6-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H147 Mn Mo6 N10 O26' _chemical_formula_weight 2199.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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 14.8991(11) _cell_length_b 16.8272(12) _cell_length_c 22.2685(17) _cell_angle_alpha 73.868(4) _cell_angle_beta 74.700(4) _cell_angle_gamma 66.883(3) _cell_volume 4856.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9782 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 26.5 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2268 _exptl_absorpt_coefficient_mu 0.946 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8789 _exptl_absorpt_correction_T_max 0.9454 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Quasar CCD' _diffrn_measurement_method '\w & \p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 69193 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.00 _reflns_number_total 19055 _reflns_number_gt 16021 _reflns_threshold_expression >2\s(I) _computing_data_collection Apex2 _computing_cell_refinement Apex2 _computing_data_reduction Apex2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics diamond3 _computing_publication_material WinGX _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^ > 2\s(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^)+(0.0271P)^2^+7.5749P] 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 none _refine_ls_number_reflns 19055 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo -0.058831(13) 0.947259(12) 0.883685(9) 0.01876(4) Uani 1 1 d . . . Mo2 Mo 0.062939(14) 1.179870(12) 0.970833(9) 0.02135(4) Uani 1 1 d . . . Mo3 Mo 0.297081(13) 0.685625(12) 0.502543(9) 0.01899(4) Uani 1 1 d . . . Mo4 Mo 0.484881(13) 0.669464(12) 0.378159(9) 0.01998(4) Uani 1 1 d . . . Mo5 Mo 0.003479(14) 1.127096(12) 0.854977(9) 0.02104(4) Uani 1 1 d . . . Mo6 Mo 0.309254(13) 0.511498(12) 0.622173(9) 0.01904(4) Uani 1 1 d . . . Mn1 Mn 0.5000 0.5000 0.5000 0.01462(9) Uani 1 2 d S . . Mn2 Mn 0.0000 1.0000 1.0000 0.01485(9) Uani 1 2 d S . . O1 O 0.06320(10) 0.98232(9) 0.91038(7) 0.0207(3) Uani 1 1 d . . . O2 O -0.09366(10) 1.07319(9) 0.86719(7) 0.0206(3) Uani 1 1 d . . . O3 O 0.01484(12) 0.92232(11) 0.81394(8) 0.0293(4) Uani 1 1 d . . . O4 O -0.17036(11) 0.94381(10) 0.88147(8) 0.0288(4) Uani 1 1 d . . . O5 O 0.11351(10) 1.02801(9) 1.01132(7) 0.0205(3) Uani 1 1 d . . . O6 O -0.00512(11) 0.83931(9) 0.94071(7) 0.0221(3) Uani 1 1 d . . . O7 O 0.17407(12) 1.18549(11) 0.97171(8) 0.0328(4) Uani 1 1 d . . . O8 O -0.01031(13) 1.28559(11) 0.94799(8) 0.0331(4) Uani 1 1 d . . . O9 O 0.05778(10) 0.87695(9) 1.03457(7) 0.0182(3) Uani 1 1 d . . . O10 O 0.09849(11) 1.13681(10) 0.89344(7) 0.0229(4) Uani 1 1 d . . . O11 O -0.07123(12) 1.23423(11) 0.83803(8) 0.0312(4) Uani 1 1 d . . . O12 O 0.07573(12) 1.10316(12) 0.78447(8) 0.0325(4) Uani 1 1 d . . . O13 O 0.52543(10) 0.37169(10) 0.51227(7) 0.0201(3) Uani 1 1 d . . . O14 O 0.35203(11) 0.67508(10) 0.41543(7) 0.0220(4) Uani 1 1 d . . . O15 O 0.29696(12) 0.78626(10) 0.50328(8) 0.0289(4) Uani 1 1 d . . . O16 O 0.17825(11) 0.70117(11) 0.50011(8) 0.0279(4) Uani 1 1 d . . . O17 O 0.34948(10) 0.53111(9) 0.51277(7) 0.0188(3) Uani 1 1 d . . . O18 O 0.30909(11) 0.62970(9) 0.58920(7) 0.0206(3) Uani 1 1 d . . . O19 O 0.51375(10) 0.51586(9) 0.40995(7) 0.0175(3) Uani 1 1 d . . . O20 O 0.19245(11) 0.51897(10) 0.62181(8) 0.0285(4) Uani 1 1 d . . . O21 O 0.31173(12) 0.50477(10) 0.69972(8) 0.0295(4) Uani 1 1 d . . . O22 O 0.37783(10) 0.39078(9) 0.61547(7) 0.0193(3) Uani 1 1 d . . . O23 O 0.48284(12) 0.66324(11) 0.30343(8) 0.0294(4) Uani 1 1 d . . . O24 O 0.48023(12) 0.77423(10) 0.37260(8) 0.0307(4) Uani 1 1 d . . . O25 O 0.48546(12) 0.29860(11) 0.35736(9) 0.0366(4) Uani 1 1 d . . . O26 O 0.30383(13) 0.73326(12) 0.91502(9) 0.0383(5) Uani 1 1 d . . . C1 C 0.31765(16) 0.49079(14) 0.47768(11) 0.0221(5) Uani 1 1 d . . . H1A H 0.2760 0.5376 0.4482 0.027 Uiso 1 1 calc R . . H1B H 0.2758 0.4582 0.5076 0.027 Uiso 1 1 calc R . . C2 C 0.46817(16) 0.34774(14) 0.48179(11) 0.0215(5) Uani 1 1 d . . . H2A H 0.4250 0.3193 0.5148 0.026 Uiso 1 1 calc R . . H2B H 0.5139 0.3040 0.4557 0.026 Uiso 1 1 calc R . . C3 C 0.46498(16) 0.47524(14) 0.38612(10) 0.0212(5) Uani 1 1 d . . . H3A H 0.5156 0.4326 0.3606 0.025 Uiso 1 1 calc R . . H3B H 0.4209 0.5212 0.3576 0.025 Uiso 1 1 calc R . . C4 C 0.40320(15) 0.42686(14) 0.43912(10) 0.0194(5) Uani 1 1 d . . . C5 C 0.39572(17) 0.33238(15) 0.37165(11) 0.0278(5) Uani 1 1 d . . . C6 C 0.32455(19) 0.30794(18) 0.34868(14) 0.0389(6) Uani 1 1 d . . . H6A H 0.3082 0.2590 0.3804 0.047 Uiso 1 1 calc R . . H6B H 0.2623 0.3591 0.3454 0.047 Uiso 1 1 calc R . . C7 C 0.3662(3) 0.2805(2) 0.28530(16) 0.0685(9) Uani 1 1 d . . . H7A H 0.3173 0.2657 0.2726 0.103 Uiso 1 1 calc R . . H7B H 0.4269 0.2288 0.2885 0.103 Uiso 1 1 calc R . . H7C H 0.3815 0.3290 0.2535 0.103 Uiso 1 1 calc R . . C8 C 0.21021(16) 0.97002(15) 0.99078(11) 0.0237(5) Uani 1 1 d . . . H8A H 0.2457 0.9431 1.0273 0.028 Uiso 1 1 calc R . . H8B H 0.2473 1.0049 0.9583 0.028 Uiso 1 1 calc R . . C9 C 0.21038(15) 0.89561(14) 0.96266(11) 0.0217(5) Uani 1 1 d . . . C10 C 0.16119(15) 0.83389(14) 1.01230(11) 0.0228(5) Uani 1 1 d . . . H10A H 0.1686 0.7844 0.9934 0.027 Uiso 1 1 calc R . . H10B H 0.1964 0.8089 1.0490 0.027 Uiso 1 1 calc R . . C11 C 0.16654(16) 0.93060(15) 0.90124(11) 0.0244(5) Uani 1 1 d . . . H11A H 0.2034 0.9669 0.8702 0.029 Uiso 1 1 calc R . . H11B H 0.1763 0.8800 0.8828 0.029 Uiso 1 1 calc R . . C12 C 0.35444(18) 0.76757(17) 0.92718(12) 0.0329(6) Uani 1 1 d . . . C13 C 0.4653(2) 0.7217(2) 0.92300(16) 0.0505(8) Uani 1 1 d . . . H13A H 0.4938 0.7581 0.9350 0.061 Uiso 1 1 calc R . . H13B H 0.4964 0.7143 0.8788 0.061 Uiso 1 1 calc R . . C14 C 0.4871(3) 0.6321(3) 0.96719(19) 0.0767(12) Uani 1 1 d . . . H14A H 0.5590 0.6029 0.9644 0.115 Uiso 1 1 calc R . . H14B H 0.4598 0.5960 0.9548 0.115 Uiso 1 1 calc R . . H14C H 0.4567 0.6397 1.0109 0.115 Uiso 1 1 calc R . . C15 C 0.9334(2) 0.0765(2) 0.68016(14) 0.0437(8) Uani 1 1 d . B . H15A H 0.9382 0.0143 0.6973 0.052 Uiso 1 1 calc R . . H15B H 0.9672 0.0920 0.7057 0.052 Uiso 1 1 calc R . . C16 C 0.9878(2) 0.0846(2) 0.61156(15) 0.0574(10) Uani 1 1 d . . . H16A H 0.9587 0.0639 0.5864 0.069 Uiso 1 1 calc R . . H16B H 0.9797 0.1472 0.5930 0.069 Uiso 1 1 calc R . . C17 C 1.0973(3) 0.0303(3) 0.6084(2) 0.0916(17) Uani 1 1 d . . . H17A H 1.1051 -0.0314 0.6300 0.110 Uiso 1 1 calc R . . H17B H 1.1273 0.0539 0.6310 0.110 Uiso 1 1 calc R . . C18 C 1.1518(4) 0.0323(5) 0.5395(2) 0.146(3) Uani 1 1 d . . . H18A H 1.2218 -0.0045 0.5389 0.219 Uiso 1 1 calc R . . H18B H 1.1466 0.0930 0.5186 0.219 Uiso 1 1 calc R . . H18C H 1.1218 0.0095 0.5169 0.219 Uiso 1 1 calc R . . C19 C 0.76981(19) 0.11488(16) 0.64885(12) 0.0346(6) Uani 1 1 d . B . H19A H 0.6991 0.1525 0.6565 0.042 Uiso 1 1 calc R . . H19B H 0.7965 0.1317 0.6034 0.042 Uiso 1 1 calc R . . C20 C 0.7761(2) 0.01955(17) 0.66232(14) 0.0420(7) Uani 1 1 d . . . H20A H 0.7566 -0.0003 0.7085 0.050 Uiso 1 1 calc R . . H20B H 0.8453 -0.0181 0.6491 0.050 Uiso 1 1 calc R . . C21 C 0.7082(2) 0.01035(19) 0.62652(15) 0.0480(8) Uani 1 1 d . . . H21A H 0.6387 0.0445 0.6424 0.058 Uiso 1 1 calc R . . H21B H 0.7241 0.0355 0.5809 0.058 Uiso 1 1 calc R . . C22 C 0.7181(3) -0.0848(2) 0.63392(19) 0.0696(10) Uani 1 1 d . . . H22A H 0.6728 -0.0877 0.6103 0.104 Uiso 1 1 calc R . . H22B H 0.7015 -0.1097 0.6790 0.104 Uiso 1 1 calc R . . H22C H 0.7864 -0.1186 0.6172 0.104 Uiso 1 1 calc R . . C23 C 0.7819(2) 0.11481(19) 0.75861(12) 0.0381(7) Uani 1 1 d . B . H23A H 0.8025 0.0501 0.7734 0.046 Uiso 1 1 calc R . . H23B H 0.8113 0.1375 0.7823 0.046 Uiso 1 1 calc R . . C24 C 0.6699(2) 0.1536(2) 0.77558(14) 0.0439(7) Uani 1 1 d . . . H24A H 0.6395 0.1183 0.7640 0.053 Uiso 1 1 calc R . . H24B H 0.6462 0.2146 0.7512 0.053 Uiso 1 1 calc R . . C25 C 0.6381(2) 0.1540(2) 0.84648(15) 0.0531(9) Uani 1 1 d . . . H25A H 0.5668 0.1616 0.8588 0.064 Uiso 1 1 calc R . . H25B H 0.6754 0.0963 0.8703 0.064 Uiso 1 1 calc R . . C26 C 0.6552(2) 0.2263(2) 0.86511(17) 0.0646(10) Uani 1 1 d . . . H26A H 0.6338 0.2232 0.9110 0.097 Uiso 1 1 calc R . . H26B H 0.6171 0.2838 0.8426 0.097 Uiso 1 1 calc R . . H26C H 0.7259 0.2185 0.8538 0.097 Uiso 1 1 calc R . . C27 C 0.8135(2) 0.23100(18) 0.66638(13) 0.0424(7) Uani 1 1 d . B . H27A H 0.7436 0.2666 0.6801 0.051 Uiso 1 1 calc R . . H27B H 0.8275 0.2445 0.6194 0.051 Uiso 1 1 calc R . . C28 C 0.8804(3) 0.2594(2) 0.69109(17) 0.0704(10) Uani 1 1 d . . . H28A H 0.8728 0.2404 0.7378 0.084 Uiso 1 1 calc R A 1 H28B H 0.9505 0.2309 0.6726 0.084 Uiso 1 1 calc R A 1 C29 C 0.8534(3) 0.3581(2) 0.67343(19) 0.0800(12) Uani 1 1 d . B 1 H29A H 0.9103 0.3737 0.6746 0.096 Uiso 1 1 calc R B 1 H29B H 0.8399 0.3787 0.6295 0.096 Uiso 1 1 calc R B 1 C30 C 0.7721(3) 0.4000(3) 0.7135(3) 0.0588(15) Uani 0.722(6) 1 d P B 1 H30A H 0.7570 0.4639 0.7004 0.088 Uiso 1 1 calc R B 1 H30B H 0.7858 0.3808 0.7569 0.088 Uiso 1 1 calc R B 1 H30C H 0.7153 0.3855 0.7119 0.088 Uiso 1 1 calc R B 1 C30' C 0.8519(9) 0.4184(8) 0.7155(6) 0.057(4) Uiso 0.278(6) 1 d P B 2 C31 C 0.3101(2) 0.3077(2) 0.77918(14) 0.0465(8) Uani 1 1 d . . . H31A H 0.2839 0.3713 0.7606 0.056 Uiso 1 1 calc R . . H31B H 0.3782 0.2835 0.7559 0.056 Uiso 1 1 calc R . . C32 C 0.3158(2) 0.2983(2) 0.84769(15) 0.0542(9) Uani 1 1 d . . . H32A H 0.3520 0.2360 0.8652 0.065 Uiso 1 1 calc R . . H32B H 0.2481 0.3152 0.8730 0.065 Uiso 1 1 calc R . . C33 C 0.3687(2) 0.3564(2) 0.85261(15) 0.0526(9) Uani 1 1 d . . . H33A H 0.4360 0.3396 0.8268 0.063 Uiso 1 1 calc R . . H33B H 0.3321 0.4185 0.8349 0.063 Uiso 1 1 calc R . . C34 C 0.3769(3) 0.3491(3) 0.92020(19) 0.0808(13) Uani 1 1 d . . . H34A H 0.4112 0.3879 0.9210 0.121 Uiso 1 1 calc R . . H34B H 0.4145 0.2881 0.9376 0.121 Uiso 1 1 calc R . . H34C H 0.3104 0.3667 0.9459 0.121 Uiso 1 1 calc R . . C35 C 0.2778(2) 0.16761(19) 0.80029(16) 0.0481(8) Uani 1 1 d . . . H35A H 0.2349 0.1408 0.7920 0.058 Uiso 1 1 calc R . . H35B H 0.2657 0.1643 0.8467 0.058 Uiso 1 1 calc R . . C36 C 0.3856(2) 0.1129(2) 0.77977(17) 0.0538(9) Uani 1 1 d . . . H36A H 0.3974 0.1105 0.7343 0.065 Uiso 1 1 calc R . . H36B H 0.4296 0.1409 0.7851 0.065 Uiso 1 1 calc R . . C37 C 0.4096(2) 0.0208(2) 0.81904(17) 0.0558(9) Uani 1 1 d . . . H37A H 0.3620 -0.0051 0.8159 0.067 Uiso 1 1 calc R . . H37B H 0.4011 0.0237 0.8641 0.067 Uiso 1 1 calc R . . C38 C 0.5145(3) -0.0392(3) 0.7983(2) 0.0764(13) Uani 1 1 d . . . H38A H 0.5262 -0.0978 0.8255 0.115 Uiso 1 1 calc R . . H38B H 0.5621 -0.0144 0.8017 0.115 Uiso 1 1 calc R . . H38C H 0.5229 -0.0439 0.7541 0.115 Uiso 1 1 calc R . . C39 C 0.1384(2) 0.30711(19) 0.79498(16) 0.0514(9) Uani 1 1 d . . . H39A H 0.1000 0.2735 0.7900 0.062 Uiso 1 1 calc R . . H39B H 0.1322 0.3028 0.8410 0.062 Uiso 1 1 calc R . . C40 C 0.0921(3) 0.4029(2) 0.76491(18) 0.0649(11) Uani 1 1 d . . . H40A H 0.0969 0.4085 0.7188 0.078 Uiso 1 1 calc R . . H40B H 0.1283 0.4380 0.7705 0.078 Uiso 1 1 calc R . . C41 C -0.0164(3) 0.4379(2) 0.7959(2) 0.0864(16) Uani 1 1 d . . . H41A H -0.0205 0.4334 0.8418 0.104 Uiso 1 1 calc R . . H41B H -0.0516 0.4012 0.7916 0.104 Uiso 1 1 calc R . . C42 C -0.0673(4) 0.5342(3) 0.7656(3) 0.126(2) Uani 1 1 d . . . H42A H -0.1373 0.5539 0.7857 0.188 Uiso 1 1 calc R . . H42B H -0.0626 0.5389 0.7201 0.188 Uiso 1 1 calc R . . H42C H -0.0347 0.5711 0.7717 0.188 Uiso 1 1 calc R . . C43 C 0.2607(2) 0.2731(2) 0.69660(15) 0.0521(8) Uani 1 1 d . . . H43A H 0.3319 0.2439 0.6807 0.063 Uiso 1 1 calc R . . H43B H 0.2438 0.3366 0.6773 0.063 Uiso 1 1 calc R . . C44 C 0.2015(3) 0.2366(3) 0.6723(2) 0.0742(11) Uani 1 1 d . . . H44A H 0.1303 0.2609 0.6903 0.089 Uiso 1 1 calc R . . H44B H 0.2238 0.1716 0.6858 0.089 Uiso 1 1 calc R . . C45 C 0.2177(3) 0.2630(4) 0.5971(2) 0.1221(14) Uani 1 1 d . . . H45A H 0.1972 0.3280 0.5847 0.147 Uiso 1 1 calc R . . H45B H 0.2893 0.2385 0.5802 0.147 Uiso 1 1 calc R . . C46 C 0.1639(5) 0.2331(4) 0.5674(3) 0.138(2) Uiso 1 1 d . . . H46A H 0.1795 0.2508 0.5211 0.207 Uiso 1 1 calc R . . H46B H 0.0925 0.2597 0.5818 0.207 Uiso 1 1 calc R . . H46C H 0.1836 0.1688 0.5791 0.207 Uiso 1 1 calc R . . C47 C 0.1884(2) 0.72944(19) 0.70887(14) 0.0439(7) Uani 1 1 d . . . H47A H 0.1833 0.6718 0.7109 0.053 Uiso 1 1 calc R . . H47B H 0.2309 0.7436 0.6680 0.053 Uiso 1 1 calc R . . C48 C 0.0858(2) 0.7989(2) 0.70914(16) 0.0588(9) Uani 1 1 d . . . H48A H 0.0884 0.8560 0.7111 0.071 Uiso 1 1 calc R . . H48B H 0.0400 0.7818 0.7471 0.071 Uiso 1 1 calc R . . C49 C 0.0470(3) 0.8089(3) 0.6482(2) 0.0820(12) Uani 1 1 d . . . H49A H -0.0108 0.8641 0.6435 0.098 Uiso 1 1 calc R . . H49B H 0.0994 0.8140 0.6109 0.098 Uiso 1 1 calc R . . C50 C 0.0181(3) 0.7361(3) 0.6489(2) 0.1045(15) Uani 1 1 d . . . H50A H -0.0043 0.7455 0.6091 0.157 Uiso 1 1 calc R . . H50B H -0.0359 0.7322 0.6847 0.157 Uiso 1 1 calc R . . H50C H 0.0749 0.6812 0.6535 0.157 Uiso 1 1 calc R . . C51 C 0.2520(2) 0.80522(17) 0.76223(13) 0.0375(7) Uani 1 1 d . . . H51A H 0.2888 0.7938 0.7966 0.045 Uiso 1 1 calc R . . H51B H 0.1854 0.8488 0.7730 0.045 Uiso 1 1 calc R . . C52 C 0.3049(2) 0.84675(18) 0.70126(13) 0.0426(7) Uani 1 1 d . . . H52A H 0.2649 0.8660 0.6673 0.051 Uiso 1 1 calc R . . H52B H 0.3697 0.8029 0.6876 0.051 Uiso 1 1 calc R . . C53 C 0.3204(3) 0.9256(2) 0.71192(16) 0.0568(9) Uani 1 1 d . . . H53A H 0.2552 0.9689 0.7258 0.068 Uiso 1 1 calc R . . H53B H 0.3596 0.9059 0.7463 0.068 Uiso 1 1 calc R . . C54 C 0.3737(3) 0.9700(2) 0.65244(19) 0.0755(12) Uani 1 1 d . . . H54A H 0.3822 1.0202 0.6614 0.113 Uiso 1 1 calc R . . H54B H 0.3345 0.9908 0.6185 0.113 Uiso 1 1 calc R . . H54C H 0.4388 0.9277 0.6390 0.113 Uiso 1 1 calc R . . C55 C 0.33919(19) 0.64746(17) 0.75186(13) 0.0366(7) Uani 1 1 d . . . H55A H 0.3274 0.5956 0.7473 0.044 Uiso 1 1 calc R . . H55B H 0.3777 0.6679 0.7110 0.044 Uiso 1 1 calc R . . C56 C 0.4026(2) 0.6174(2) 0.80225(14) 0.0448(8) Uani 1 1 d . . . H56A H 0.3647 0.5992 0.8441 0.054 Uiso 1 1 calc R . . H56B H 0.4215 0.6665 0.8047 0.054 Uiso 1 1 calc R . . C57 C 0.4952(2) 0.54028(18) 0.78602(13) 0.0404(7) Uani 1 1 d . . . H57A H 0.4753 0.4930 0.7813 0.049 Uiso 1 1 calc R . . H57B H 0.5335 0.5598 0.7448 0.049 Uiso 1 1 calc R . . C58 C 0.5611(3) 0.5032(2) 0.83601(16) 0.0600(10) Uani 1 1 d . . . H58A H 0.6195 0.4539 0.8232 0.090 Uiso 1 1 calc R . . H58B H 0.5242 0.4826 0.8768 0.090 Uiso 1 1 calc R . . H58C H 0.5824 0.5494 0.8403 0.090 Uiso 1 1 calc R . . C59 C 0.1784(2) 0.69684(19) 0.82693(13) 0.0426(7) Uani 1 1 d . . . H59A H 0.2151 0.6900 0.8602 0.051 Uiso 1 1 calc R . . H59B H 0.1154 0.7469 0.8324 0.051 Uiso 1 1 calc R . . C60 C 0.1540(2) 0.6141(2) 0.83783(16) 0.0550(9) Uani 1 1 d . . . H60A H 0.1005 0.6263 0.8145 0.066 Uiso 1 1 calc R . . H60B H 0.2132 0.5674 0.8211 0.066 Uiso 1 1 calc R . . C61 C 0.1214(4) 0.5823(3) 0.9078(2) 0.0951(16) Uani 1 1 d . . . H61A H 0.0655 0.6311 0.9248 0.114 Uiso 1 1 calc R . . H61B H 0.1768 0.5670 0.9304 0.114 Uiso 1 1 calc R . . C62 C 0.0892(4) 0.5027(4) 0.9216(3) 0.122(2) Uani 1 1 d . . . H62A H 0.0709 0.4846 0.9676 0.183 Uiso 1 1 calc R . . H62B H 0.1440 0.4541 0.9048 0.183 Uiso 1 1 calc R . . H62C H 0.0320 0.5182 0.9014 0.183 Uiso 1 1 calc R . . C71 C 0.4576(2) 0.11847(19) 0.49475(16) 0.0487(8) Uani 1 1 d . . . C72 C 0.5492(3) 0.1081(2) 0.5114(2) 0.0705(11) Uani 1 1 d . . . H72A H 0.5882 0.0453 0.5213 0.106 Uiso 1 1 calc R . . H72B H 0.5348 0.1343 0.5486 0.106 Uiso 1 1 calc R . . H72C H 0.5868 0.1377 0.4756 0.106 Uiso 1 1 calc R . . C73 C 0.0576(2) 0.42492(19) 0.44995(15) 0.0444(8) Uani 1 1 d . . . C74 C -0.0266(2) 0.3947(2) 0.46808(19) 0.0625(10) Uani 1 1 d . . . H74A H -0.0028 0.3308 0.4708 0.094 Uiso 1 1 calc R . . H74B H -0.0698 0.4242 0.4362 0.094 Uiso 1 1 calc R . . H74C H -0.0638 0.4087 0.5095 0.094 Uiso 1 1 calc R . . C75 C 0.5430(2) 0.9034(2) 0.97188(18) 0.0593(10) Uani 1 1 d . . . C76 C 0.6423(4) 0.9091(3) 0.9591(3) 0.1059(17) Uiso 1 1 d . . . H76A H 0.6460 0.9590 0.9243 0.159 Uiso 1 1 calc R . . H76B H 0.6918 0.8545 0.9470 0.159 Uiso 1 1 calc R . . H76C H 0.6554 0.9176 0.9973 0.159 Uiso 1 1 calc R . . C77 C -0.2284(3) 0.4921(3) 0.9312(2) 0.0874(13) Uiso 1 1 d . . . C78 C -0.2329(3) 0.4082(3) 0.9346(2) 0.0809(12) Uiso 1 1 d . C . H78A H -0.2705 0.4127 0.9030 0.121 Uiso 1 1 calc R . . H78B H -0.2658 0.3879 0.9771 0.121 Uiso 1 1 calc R . . H78C H -0.1656 0.3661 0.9261 0.121 Uiso 1 1 calc R . . C79 C -0.1883(5) 0.7806(4) 0.8348(3) 0.124(2) Uiso 1 1 d D . . C80 C -0.1380(4) 0.7296(4) 0.8905(3) 0.1185(19) Uiso 1 1 d . D . H80A H -0.0666 0.7036 0.8757 0.178 Uiso 1 1 calc R . . H80B H -0.1648 0.6827 0.9134 0.178 Uiso 1 1 calc R . . H80C H -0.1495 0.7692 0.9189 0.178 Uiso 1 1 calc R . . N1 N 0.31635(13) 0.84455(13) 0.94731(9) 0.0263(5) Uani 1 1 d . . . H1 H 0.3587 0.8663 0.9517 0.032 Uiso 1 1 calc R . . N2 N 0.35225(13) 0.39332(12) 0.40900(9) 0.0232(4) Uani 1 1 d . . . H2 H 0.2871 0.4150 0.4159 0.028 Uiso 1 1 calc R . . N3 N 0.23909(16) 0.72027(14) 0.76239(10) 0.0356(5) Uani 1 1 d . . . N4 N 0.24713(17) 0.26354(15) 0.76786(12) 0.0457(7) Uani 1 1 d . . . N5 N 0.82513(16) 0.13417(14) 0.68830(10) 0.0341(5) Uani 1 1 d . . . N6 N 0.3870(2) 0.1259(2) 0.48140(17) 0.0745(9) Uani 1 1 d . . . N7 N 0.12276(19) 0.44827(19) 0.43725(16) 0.0636(9) Uani 1 1 d . . . N8 N 0.4688(2) 0.8996(2) 0.97994(16) 0.0694(9) Uani 1 1 d . . . N9 N -0.2085(5) 0.5490(5) 0.9375(4) 0.082(2) Uiso 0.50 1 d P C 1 N10 N -0.2402(9) 0.8222(10) 0.7975(7) 0.112(5) Uiso 0.312(12) 1 d PDU D 1 N9' N -0.2471(6) 0.5744(6) 0.9133(4) 0.097(3) Uiso 0.50 1 d P C 2 N10' N -0.2009(10) 0.8257(9) 0.7844(5) 0.105(5) Uiso 0.338(12) 1 d PDU D 2 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 0.02104(8) 0.01982(8) 0.01643(9) -0.00350(7) -0.00345(7) -0.00802(7) Mo2 0.02642(9) 0.02063(8) 0.01980(9) 0.00003(7) -0.00446(7) -0.01347(7) Mo3 0.01762(8) 0.01661(8) 0.01900(9) -0.00088(7) -0.00099(7) -0.00522(7) Mo4 0.01884(8) 0.01828(8) 0.01794(9) 0.00255(7) -0.00040(7) -0.00726(7) Mo5 0.02509(9) 0.02361(9) 0.01599(9) 0.00182(7) -0.00414(7) -0.01355(7) Mo6 0.02021(9) 0.01804(8) 0.01608(9) -0.00179(7) 0.00175(7) -0.00790(7) Mn1 0.01515(19) 0.01416(19) 0.0137(2) -0.00063(16) -0.00086(16) -0.00670(16) Mn2 0.01482(19) 0.01629(19) 0.0133(2) -0.00182(16) -0.00066(16) -0.00707(16) O1 0.0156(7) 0.0198(7) 0.0247(8) -0.0030(6) -0.0023(6) -0.0056(6) O2 0.0219(7) 0.0216(7) 0.0196(7) -0.0007(6) -0.0053(6) -0.0099(6) O3 0.0324(8) 0.0299(8) 0.0215(8) -0.0076(7) -0.0017(7) -0.0067(7) O4 0.0255(8) 0.0272(8) 0.0360(9) -0.0030(7) -0.0102(7) -0.0105(7) O5 0.0189(7) 0.0196(7) 0.0187(7) -0.0023(6) 0.0006(6) -0.0056(6) O6 0.0253(7) 0.0190(7) 0.0220(8) -0.0038(6) -0.0045(6) -0.0076(6) O7 0.0353(8) 0.0436(9) 0.0284(9) -0.0042(7) -0.0048(7) -0.0253(7) O8 0.0449(9) 0.0242(8) 0.0310(9) 0.0004(7) -0.0119(8) -0.0134(7) O9 0.0179(7) 0.0198(7) 0.0166(7) -0.0032(6) -0.0013(6) -0.0074(6) O10 0.0251(7) 0.0288(7) 0.0177(7) 0.0000(6) -0.0012(6) -0.0169(6) O11 0.0383(9) 0.0275(8) 0.0293(9) 0.0036(7) -0.0132(7) -0.0146(7) O12 0.0357(8) 0.0444(9) 0.0208(8) -0.0031(7) 0.0003(7) -0.0229(7) O13 0.0188(7) 0.0248(7) 0.0180(7) -0.0034(6) -0.0018(6) -0.0105(6) O14 0.0207(7) 0.0210(7) 0.0209(8) 0.0016(6) -0.0041(6) -0.0072(6) O15 0.0317(8) 0.0212(7) 0.0327(9) -0.0024(7) -0.0037(7) -0.0113(7) O16 0.0214(7) 0.0319(8) 0.0277(9) -0.0044(7) -0.0012(7) -0.0095(7) O17 0.0234(7) 0.0183(7) 0.0162(7) -0.0026(6) -0.0022(6) -0.0099(6) O18 0.0228(7) 0.0180(7) 0.0195(7) -0.0043(6) 0.0008(6) -0.0077(6) O19 0.0176(6) 0.0188(7) 0.0171(7) -0.0027(6) -0.0019(6) -0.0087(6) O20 0.0221(8) 0.0264(8) 0.0326(9) -0.0040(7) 0.0022(7) -0.0095(6) O21 0.0409(9) 0.0258(8) 0.0189(8) -0.0034(6) -0.0004(7) -0.0122(7) O22 0.0183(7) 0.0182(7) 0.0188(7) 0.0010(6) 0.0018(6) -0.0099(6) O23 0.0256(8) 0.0340(9) 0.0205(8) 0.0014(7) -0.0018(7) -0.0080(7) O24 0.0280(8) 0.0214(8) 0.0365(10) 0.0004(7) -0.0001(7) -0.0097(7) O25 0.0296(9) 0.0414(9) 0.0437(10) -0.0244(8) -0.0002(8) -0.0105(7) O26 0.0302(9) 0.0436(9) 0.0436(10) -0.0261(8) -0.0079(8) -0.0025(8) C1 0.0218(10) 0.0230(10) 0.0251(11) -0.0068(9) -0.0030(9) -0.0107(8) C2 0.0218(10) 0.0216(10) 0.0243(11) -0.0047(8) -0.0043(9) -0.0104(8) C3 0.0251(10) 0.0247(10) 0.0174(10) -0.0041(8) -0.0032(8) -0.0127(9) C4 0.0201(9) 0.0216(10) 0.0199(10) -0.0051(8) -0.0019(8) -0.0110(8) C5 0.0316(12) 0.0290(11) 0.0275(12) -0.0079(9) -0.0056(10) -0.0135(10) C6 0.0390(13) 0.0389(13) 0.0509(15) -0.0186(12) -0.0131(12) -0.0161(11) C7 0.094(2) 0.098(2) 0.0514(18) -0.0324(16) -0.0071(17) -0.0646(18) C8 0.0162(10) 0.0278(11) 0.0255(11) -0.0067(9) 0.0004(9) -0.0073(9) C9 0.0134(9) 0.0259(10) 0.0221(11) -0.0075(9) 0.0006(8) -0.0035(8) C10 0.0166(10) 0.0208(10) 0.0253(11) -0.0038(9) -0.0010(9) -0.0026(8) C11 0.0168(10) 0.0308(11) 0.0215(11) -0.0061(9) 0.0017(9) -0.0064(9) C12 0.0251(12) 0.0409(13) 0.0283(12) -0.0158(11) -0.0034(10) -0.0017(11) C13 0.0237(13) 0.0619(17) 0.0664(18) -0.0397(15) -0.0070(13) 0.0023(13) C14 0.0520(19) 0.072(2) 0.084(2) -0.030(2) -0.0347(18) 0.0265(18) C15 0.0346(14) 0.0468(16) 0.0412(16) 0.0039(13) -0.0148(12) -0.0087(12) C16 0.0436(17) 0.073(2) 0.0427(18) -0.0010(16) -0.0072(14) -0.0137(16) C17 0.048(2) 0.119(4) 0.069(3) 0.000(3) 0.002(2) -0.009(2) C18 0.062(3) 0.242(8) 0.082(4) -0.035(4) 0.016(3) -0.015(4) C19 0.0412(13) 0.0305(12) 0.0314(13) -0.0016(10) -0.0169(11) -0.0079(11) C20 0.0461(15) 0.0283(13) 0.0467(16) -0.0022(12) -0.0163(13) -0.0059(12) C21 0.0627(17) 0.0365(14) 0.0480(17) -0.0064(13) -0.0183(14) -0.0162(13) C22 0.105(3) 0.0443(17) 0.073(2) -0.0057(16) -0.030(2) -0.0355(18) C23 0.0419(14) 0.0393(14) 0.0275(13) 0.0012(11) -0.0156(11) -0.0074(12) C24 0.0383(14) 0.0516(16) 0.0387(15) -0.0062(13) -0.0136(12) -0.0096(13) C25 0.0472(17) 0.0583(19) 0.0399(17) -0.0083(14) -0.0089(14) -0.0037(15) C26 0.0501(18) 0.080(2) 0.061(2) -0.0309(18) -0.0187(16) -0.0016(17) C27 0.0623(16) 0.0331(13) 0.0351(14) 0.0039(11) -0.0258(13) -0.0161(12) C28 0.117(2) 0.0599(19) 0.0582(19) 0.0114(15) -0.0553(18) -0.0457(18) C29 0.142(3) 0.062(2) 0.060(2) 0.0032(17) -0.042(2) -0.055(2) C30 0.049(3) 0.040(2) 0.081(4) 0.000(2) -0.023(2) -0.010(2) C31 0.0551(16) 0.0471(15) 0.0382(16) 0.0003(12) 0.0085(13) -0.0352(13) C32 0.0612(19) 0.0554(18) 0.0384(17) -0.0013(14) 0.0084(15) -0.0285(15) C33 0.0602(19) 0.0467(17) 0.0446(18) -0.0041(14) -0.0062(15) -0.0170(15) C34 0.086(3) 0.097(3) 0.058(2) -0.018(2) -0.014(2) -0.028(2) C35 0.0425(15) 0.0387(14) 0.0556(19) -0.0031(13) 0.0128(14) -0.0239(12) C36 0.0395(15) 0.0511(17) 0.062(2) -0.0117(15) 0.0169(15) -0.0232(13) C37 0.0430(16) 0.0509(17) 0.067(2) -0.0145(16) 0.0133(15) -0.0219(14) C38 0.049(2) 0.065(2) 0.094(3) -0.016(2) 0.010(2) -0.0127(18) C39 0.0410(15) 0.0414(15) 0.056(2) 0.0067(14) 0.0114(14) -0.0214(13) C40 0.065(2) 0.0419(17) 0.064(2) 0.0128(16) 0.0111(18) -0.0236(15) C41 0.071(3) 0.047(2) 0.091(3) 0.019(2) 0.015(2) -0.0081(19) C42 0.103(4) 0.057(3) 0.126(4) 0.032(3) 0.017(3) 0.009(3) C43 0.0525(16) 0.0625(17) 0.0478(18) -0.0062(14) 0.0090(14) -0.0408(14) C44 0.0655(19) 0.091(2) 0.086(3) -0.023(2) 0.0084(19) -0.0579(17) C45 0.110(2) 0.242(4) 0.095(3) -0.095(3) 0.036(2) -0.137(2) C47 0.0397(14) 0.0499(15) 0.0415(14) -0.0276(12) -0.0101(12) -0.0002(13) C48 0.0441(17) 0.0670(19) 0.0617(18) -0.0406(15) -0.0177(14) 0.0088(15) C49 0.061(2) 0.084(2) 0.100(3) -0.060(2) -0.0423(19) 0.0238(19) C50 0.081(3) 0.101(3) 0.143(4) -0.071(3) -0.057(3) 0.013(2) C51 0.0349(13) 0.0384(13) 0.0353(13) -0.0204(11) -0.0053(11) -0.0002(11) C52 0.0389(15) 0.0433(15) 0.0378(15) -0.0173(12) -0.0055(12) -0.0004(12) C53 0.067(2) 0.0433(16) 0.0552(19) -0.0164(14) -0.0034(16) -0.0143(15) C54 0.098(3) 0.059(2) 0.071(3) -0.0146(18) -0.001(2) -0.036(2) C55 0.0325(13) 0.0391(13) 0.0350(13) -0.0209(11) -0.0030(11) -0.0016(11) C56 0.0385(15) 0.0501(16) 0.0412(15) -0.0235(13) -0.0090(12) 0.0007(13) C57 0.0391(14) 0.0398(14) 0.0375(14) -0.0140(12) -0.0064(12) -0.0043(12) C58 0.059(2) 0.0563(19) 0.0497(19) -0.0120(15) -0.0189(16) 0.0026(16) C59 0.0395(14) 0.0524(15) 0.0363(14) -0.0230(12) 0.0029(12) -0.0127(13) C60 0.0470(17) 0.0569(18) 0.059(2) -0.0258(15) 0.0069(15) -0.0159(15) C61 0.105(3) 0.100(3) 0.073(3) -0.010(2) 0.015(3) -0.053(3) C62 0.107(4) 0.114(4) 0.123(5) -0.015(3) 0.025(3) -0.050(3) C71 0.0575(17) 0.0386(14) 0.0562(18) -0.0108(13) -0.0129(15) -0.0202(13) C72 0.0636(19) 0.0437(16) 0.120(3) -0.0276(18) -0.040(2) -0.0115(15) C73 0.0308(13) 0.0443(15) 0.0583(18) -0.0102(13) -0.0123(13) -0.0102(12) C74 0.0455(16) 0.079(2) 0.079(2) -0.0198(18) -0.0124(16) -0.0339(15) C75 0.0440(16) 0.072(2) 0.064(2) -0.0022(17) -0.0176(15) -0.0250(16) N1 0.0151(8) 0.0334(10) 0.0306(10) -0.0127(8) -0.0021(8) -0.0055(8) N2 0.0187(8) 0.0280(9) 0.0279(10) -0.0102(8) -0.0040(7) -0.0100(7) N3 0.0317(11) 0.0418(11) 0.0320(11) -0.0209(9) -0.0036(9) -0.0035(9) N4 0.0456(12) 0.0413(12) 0.0466(15) -0.0008(11) 0.0129(11) -0.0299(10) N5 0.0390(11) 0.0322(11) 0.0277(11) 0.0021(9) -0.0161(9) -0.0077(9) N6 0.0670(17) 0.084(2) 0.089(2) -0.0245(17) -0.0259(17) -0.0312(16) N7 0.0321(13) 0.0664(16) 0.096(2) -0.0251(16) 0.0022(14) -0.0236(12) N8 0.0439(14) 0.0889(19) 0.093(2) -0.0237(17) -0.0134(15) -0.0362(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O4 1.6992(17) . ? Mo1 O3 1.7012(16) . ? Mo1 O6 1.9146(15) . ? Mo1 O2 1.9234(15) . ? Mo1 O5 2.3608(15) 2_577 ? Mo1 O1 2.3697(16) . ? Mo2 O8 1.6971(16) . ? Mo2 O7 1.7005(17) . ? Mo2 O10 1.9200(16) . ? Mo2 O6 1.9226(15) 2_577 ? Mo2 O5 2.3403(14) . ? Mo2 O9 2.3858(15) 2_577 ? Mo3 O15 1.6973(17) . ? Mo3 O16 1.6985(16) . ? Mo3 O18 1.9189(15) . ? Mo3 O14 1.9246(15) . ? Mo3 O17 2.3648(14) . ? Mo3 O13 2.3970(14) 2_666 ? Mo4 O23 1.7051(17) . ? Mo4 O24 1.7074(17) . ? Mo4 O14 1.9093(15) . ? Mo4 O22 1.9175(14) 2_666 ? Mo4 O13 2.3246(15) 2_666 ? Mo4 O19 2.3745(14) . ? Mo5 O11 1.7027(16) . ? Mo5 O12 1.7044(16) . ? Mo5 O10 1.9141(16) . ? Mo5 O2 1.9177(16) . ? Mo5 O1 2.3358(14) . ? Mo5 O9 2.3788(14) 2_577 ? Mo6 O20 1.6969(17) . ? Mo6 O21 1.7081(17) . ? Mo6 O22 1.9107(14) . ? Mo6 O18 1.9186(15) . ? Mo6 O17 2.3111(15) . ? Mo6 O19 2.4315(14) 2_666 ? Mn1 O19 1.9139(14) 2_666 ? Mn1 O19 1.9139(14) . ? Mn1 O13 1.9910(15) 2_666 ? Mn1 O13 1.9910(15) . ? Mn1 O17 2.0515(14) 2_666 ? Mn1 O17 2.0515(14) . ? Mn2 O9 1.9197(14) 2_577 ? Mn2 O9 1.9197(14) . ? Mn2 O5 2.0156(16) . ? Mn2 O5 2.0156(16) 2_577 ? Mn2 O1 2.0189(15) 2_577 ? Mn2 O1 2.0189(15) . ? O1 C11 1.432(2) . ? O5 C8 1.426(2) . ? O5 Mo1 2.3608(15) 2_577 ? O6 Mo2 1.9226(15) 2_577 ? O9 C10 1.437(2) . ? O9 Mo5 2.3788(14) 2_577 ? O9 Mo2 2.3858(15) 2_577 ? O13 C2 1.442(3) . ? O13 Mo4 2.3246(15) 2_666 ? O13 Mo3 2.3970(14) 2_666 ? O17 C1 1.428(3) . ? O19 C3 1.439(3) . ? O19 Mo6 2.4315(14) 2_666 ? O22 Mo4 1.9175(14) 2_666 ? O25 C5 1.221(3) . ? O26 C12 1.229(3) . ? C1 C4 1.542(3) . ? C2 C4 1.544(3) . ? C3 C4 1.544(3) . ? C4 N2 1.470(3) . ? C5 N2 1.353(3) . ? C5 C6 1.517(4) . ? C6 C7 1.505(4) . ? C8 C9 1.547(3) . ? C9 N1 1.470(3) . ? C9 C11 1.538(3) . ? C9 C10 1.539(3) . ? C12 N1 1.346(3) . ? C12 C13 1.514(4) . ? C13 C14 1.518(5) . ? C15 N5 1.514(3) . ? C15 C16 1.525(4) . ? C16 C17 1.519(5) . ? C17 C18 1.534(6) . ? C19 C20 1.517(4) . ? C19 N5 1.519(4) . ? C20 C21 1.517(4) . ? C21 C22 1.514(4) . ? C23 C24 1.518(4) . ? C23 N5 1.523(3) . ? C24 C25 1.525(4) . ? C25 C26 1.515(5) . ? C27 N5 1.518(3) . ? C27 C28 1.528(5) . ? C28 C29 1.506(5) . ? C29 C30 1.368(6) . ? C31 N4 1.508(4) . ? C31 C32 1.511(4) . ? C32 C33 1.516(5) . ? C33 C34 1.510(5) . ? C35 N4 1.511(4) . ? C35 C36 1.523(4) . ? C36 C37 1.507(4) . ? C37 C38 1.521(4) . ? C39 C40 1.514(4) . ? C39 N4 1.525(4) . ? C40 C41 1.526(5) . ? C41 C42 1.534(5) . ? C43 N4 1.516(4) . ? C43 C44 1.519(5) . ? C44 C45 1.587(6) . ? C45 C46 1.454(8) . ? C47 N3 1.515(4) . ? C47 C48 1.516(4) . ? C48 C49 1.554(5) . ? C49 C50 1.444(6) . ? C51 N3 1.514(4) . ? C51 C52 1.515(4) . ? C52 C53 1.521(5) . ? C53 C54 1.518(5) . ? C55 C56 1.509(4) . ? C55 N3 1.523(3) . ? C56 C57 1.519(4) . ? C57 C58 1.518(4) . ? C59 C60 1.513(5) . ? C59 N3 1.523(3) . ? C60 C61 1.513(5) . ? C61 C62 1.522(7) . ? C71 N6 1.119(4) . ? C71 C72 1.440(5) . ? C73 N7 1.127(4) . ? C73 C74 1.454(4) . ? C75 N8 1.096(4) . ? C75 C76 1.467(6) . ? C77 N9 1.160(9) . ? C77 N9' 1.266(9) . ? C77 C78 1.418(6) . ? C79 N10 1.170(12) . ? C79 N10' 1.181(12) . ? C79 C80 1.494(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mo1 O3 105.59(9) . . ? O4 Mo1 O6 102.12(7) . . ? O3 Mo1 O6 100.09(7) . . ? O4 Mo1 O2 98.24(7) . . ? O3 Mo1 O2 101.55(7) . . ? O6 Mo1 O2 144.93(7) . . ? O4 Mo1 O5 91.38(7) . 2_577 ? O3 Mo1 O5 162.39(7) . 2_577 ? O6 Mo1 O5 71.15(6) . 2_577 ? O2 Mo1 O5 80.16(6) . 2_577 ? O4 Mo1 O1 161.26(7) . . ? O3 Mo1 O1 91.67(7) . . ? O6 Mo1 O1 81.51(6) . . ? O2 Mo1 O1 70.61(6) . . ? O5 Mo1 O1 72.21(5) 2_577 . ? O8 Mo2 O7 105.35(9) . . ? O8 Mo2 O10 101.23(8) . . ? O7 Mo2 O10 98.38(7) . . ? O8 Mo2 O6 99.38(7) . 2_577 ? O7 Mo2 O6 103.33(8) . 2_577 ? O10 Mo2 O6 144.75(7) . 2_577 ? O8 Mo2 O5 161.19(7) . . ? O7 Mo2 O5 92.91(7) . . ? O10 Mo2 O5 80.04(6) . . ? O6 Mo2 O5 71.50(6) 2_577 . ? O8 Mo2 O9 92.43(7) . 2_577 ? O7 Mo2 O9 160.71(7) . 2_577 ? O10 Mo2 O9 70.31(6) . 2_577 ? O6 Mo2 O9 80.56(6) 2_577 2_577 ? O5 Mo2 O9 70.16(5) . 2_577 ? O15 Mo3 O16 105.37(8) . . ? O15 Mo3 O18 99.53(7) . . ? O16 Mo3 O18 103.21(7) . . ? O15 Mo3 O14 102.34(7) . . ? O16 Mo3 O14 97.51(7) . . ? O18 Mo3 O14 144.53(6) . . ? O15 Mo3 O17 160.39(7) . . ? O16 Mo3 O17 93.55(7) . . ? O18 Mo3 O17 70.57(6) . . ? O14 Mo3 O17 79.77(6) . . ? O15 Mo3 O13 90.46(7) . 2_666 ? O16 Mo3 O13 161.79(7) . 2_666 ? O18 Mo3 O13 82.51(6) . 2_666 ? O14 Mo3 O13 69.80(6) . 2_666 ? O17 Mo3 O13 71.80(5) . 2_666 ? O23 Mo4 O24 105.43(8) . . ? O23 Mo4 O14 98.05(7) . . ? O24 Mo4 O14 102.74(7) . . ? O23 Mo4 O22 102.34(7) . 2_666 ? O24 Mo4 O22 98.22(7) . 2_666 ? O14 Mo4 O22 145.56(6) . 2_666 ? O23 Mo4 O13 157.87(7) . 2_666 ? O24 Mo4 O13 96.08(7) . 2_666 ? O14 Mo4 O13 71.72(6) . 2_666 ? O22 Mo4 O13 79.19(6) 2_666 2_666 ? O23 Mo4 O19 88.97(7) . . ? O24 Mo4 O19 164.02(7) . . ? O14 Mo4 O19 81.58(6) . . ? O22 Mo4 O19 71.42(6) 2_666 . ? O13 Mo4 O19 70.42(5) 2_666 . ? O11 Mo5 O12 105.67(8) . . ? O11 Mo5 O10 101.58(8) . . ? O12 Mo5 O10 99.74(8) . . ? O11 Mo5 O2 98.08(7) . . ? O12 Mo5 O2 102.94(8) . . ? O10 Mo5 O2 144.55(6) . . ? O11 Mo5 O1 159.73(7) . . ? O12 Mo5 O1 93.77(7) . . ? O10 Mo5 O1 80.22(6) . . ? O2 Mo5 O1 71.49(6) . . ? O11 Mo5 O9 90.62(7) . 2_577 ? O12 Mo5 O9 162.66(7) . 2_577 ? O10 Mo5 O9 70.56(6) . 2_577 ? O2 Mo5 O9 80.09(6) . 2_577 ? O1 Mo5 O9 70.77(5) . 2_577 ? O20 Mo6 O21 104.91(8) . . ? O20 Mo6 O22 99.38(7) . . ? O21 Mo6 O22 100.07(7) . . ? O20 Mo6 O18 104.07(7) . . ? O21 Mo6 O18 98.69(7) . . ? O22 Mo6 O18 144.91(6) . . ? O20 Mo6 O17 92.13(7) . . ? O21 Mo6 O17 162.24(7) . . ? O22 Mo6 O17 81.65(6) . . ? O18 Mo6 O17 71.82(6) . . ? O20 Mo6 O19 160.85(7) . 2_666 ? O21 Mo6 O19 92.95(7) . 2_666 ? O22 Mo6 O19 70.19(6) . 2_666 ? O18 Mo6 O19 79.49(5) . 2_666 ? O17 Mo6 O19 70.86(5) . 2_666 ? O19 Mn1 O19 180.000(1) 2_666 . ? O19 Mn1 O13 92.15(6) 2_666 2_666 ? O19 Mn1 O13 87.85(6) . 2_666 ? O19 Mn1 O13 87.85(6) 2_666 . ? O19 Mn1 O13 92.15(6) . . ? O13 Mn1 O13 180.00(9) 2_666 . ? O19 Mn1 O17 92.21(6) 2_666 2_666 ? O19 Mn1 O17 87.79(6) . 2_666 ? O13 Mn1 O17 92.63(6) 2_666 2_666 ? O13 Mn1 O17 87.37(6) . 2_666 ? O19 Mn1 O17 87.79(6) 2_666 . ? O19 Mn1 O17 92.21(6) . . ? O13 Mn1 O17 87.37(6) 2_666 . ? O13 Mn1 O17 92.63(6) . . ? O17 Mn1 O17 180.00(8) 2_666 . ? O9 Mn2 O9 180.00(9) 2_577 . ? O9 Mn2 O5 87.26(6) 2_577 . ? O9 Mn2 O5 92.74(6) . . ? O9 Mn2 O5 92.74(6) 2_577 2_577 ? O9 Mn2 O5 87.26(6) . 2_577 ? O5 Mn2 O5 180.000(1) . 2_577 ? O9 Mn2 O1 92.26(6) 2_577 2_577 ? O9 Mn2 O1 87.74(6) . 2_577 ? O5 Mn2 O1 87.41(6) . 2_577 ? O5 Mn2 O1 92.59(6) 2_577 2_577 ? O9 Mn2 O1 87.74(6) 2_577 . ? O9 Mn2 O1 92.26(6) . . ? O5 Mn2 O1 92.59(6) . . ? O5 Mn2 O1 87.41(6) 2_577 . ? O1 Mn2 O1 180.000(1) 2_577 . ? C11 O1 Mn2 115.66(13) . . ? C11 O1 Mo5 121.66(13) . . ? Mn2 O1 Mo5 99.98(6) . . ? C11 O1 Mo1 123.38(14) . . ? Mn2 O1 Mo1 99.99(6) . . ? Mo5 O1 Mo1 90.90(5) . . ? Mo5 O2 Mo1 121.63(7) . . ? C8 O5 Mn2 115.64(14) . . ? C8 O5 Mo2 121.93(13) . . ? Mn2 O5 Mo2 100.61(6) . . ? C8 O5 Mo1 122.35(13) . 2_577 ? Mn2 O5 Mo1 100.38(6) . 2_577 ? Mo2 O5 Mo1 90.89(5) . 2_577 ? Mo1 O6 Mo2 121.63(7) . 2_577 ? C10 O9 Mn2 117.60(12) . . ? C10 O9 Mo5 120.30(12) . 2_577 ? Mn2 O9 Mo5 101.51(6) . 2_577 ? C10 O9 Mo2 120.57(13) . 2_577 ? Mn2 O9 Mo2 101.97(6) . 2_577 ? Mo5 O9 Mo2 89.88(5) 2_577 2_577 ? Mo5 O10 Mo2 122.75(8) . . ? C2 O13 Mn1 116.31(12) . . ? C2 O13 Mo4 119.57(12) . 2_666 ? Mn1 O13 Mo4 100.55(6) . 2_666 ? C2 O13 Mo3 123.74(12) . 2_666 ? Mn1 O13 Mo3 100.77(6) . 2_666 ? Mo4 O13 Mo3 90.80(5) 2_666 2_666 ? Mo4 O14 Mo3 122.57(9) . . ? C1 O17 Mn1 115.16(12) . . ? C1 O17 Mo6 121.89(12) . . ? Mn1 O17 Mo6 100.61(6) . . ? C1 O17 Mo3 122.70(12) . . ? Mn1 O17 Mo3 100.04(6) . . ? Mo6 O17 Mo3 91.48(5) . . ? Mo6 O18 Mo3 121.54(8) . . ? C3 O19 Mn1 118.14(12) . . ? C3 O19 Mo4 120.82(12) . . ? Mn1 O19 Mo4 101.17(6) . . ? C3 O19 Mo6 121.46(11) . 2_666 ? Mn1 O19 Mo6 100.65(6) . 2_666 ? Mo4 O19 Mo6 88.99(5) . 2_666 ? Mo6 O22 Mo4 123.26(8) . 2_666 ? O17 C1 C4 114.05(17) . . ? O13 C2 C4 113.40(18) . . ? O19 C3 C4 113.24(17) . . ? N2 C4 C1 103.66(17) . . ? N2 C4 C2 107.99(17) . . ? C1 C4 C2 112.45(18) . . ? N2 C4 C3 108.14(18) . . ? C1 C4 C3 111.76(17) . . ? C2 C4 C3 112.32(17) . . ? O25 C5 N2 123.2(2) . . ? O25 C5 C6 121.7(2) . . ? N2 C5 C6 115.0(2) . . ? C7 C6 C5 112.8(2) . . ? O5 C8 C9 113.89(18) . . ? N1 C9 C11 108.69(17) . . ? N1 C9 C10 107.43(17) . . ? C11 C9 C10 112.3(2) . . ? N1 C9 C8 103.32(18) . . ? C11 C9 C8 112.74(19) . . ? C10 C9 C8 111.78(18) . . ? O9 C10 C9 113.41(17) . . ? O1 C11 C9 113.65(17) . . ? O26 C12 N1 123.5(2) . . ? O26 C12 C13 120.6(2) . . ? N1 C12 C13 115.8(2) . . ? C12 C13 C14 109.9(3) . . ? N5 C15 C16 114.2(2) . . ? C17 C16 C15 110.6(3) . . ? C16 C17 C18 111.3(4) . . ? C20 C19 N5 114.7(2) . . ? C19 C20 C21 110.0(2) . . ? C22 C21 C20 112.2(3) . . ? C24 C23 N5 115.6(2) . . ? C23 C24 C25 110.5(2) . . ? C26 C25 C24 113.1(3) . . ? N5 C27 C28 114.8(2) . . ? C29 C28 C27 110.1(3) . . ? C30 C29 C28 112.0(4) . . ? N4 C31 C32 116.1(2) . . ? C31 C32 C33 110.2(3) . . ? C34 C33 C32 112.4(3) . . ? N4 C35 C36 115.2(2) . . ? C37 C36 C35 110.3(2) . . ? C36 C37 C38 113.0(3) . . ? C40 C39 N4 115.1(2) . . ? C39 C40 C41 109.7(3) . . ? C40 C41 C42 111.6(3) . . ? N4 C43 C44 117.5(3) . . ? C43 C44 C45 108.9(3) . . ? C46 C45 C44 114.9(4) . . ? N3 C47 C48 115.3(2) . . ? C47 C48 C49 110.2(2) . . ? C50 C49 C48 113.3(4) . . ? N3 C51 C52 117.0(2) . . ? C51 C52 C53 109.6(2) . . ? C54 C53 C52 112.2(3) . . ? C56 C55 N3 117.2(2) . . ? C55 C56 C57 109.5(2) . . ? C58 C57 C56 112.9(2) . . ? C60 C59 N3 115.7(2) . . ? C61 C60 C59 111.0(3) . . ? C60 C61 C62 113.7(4) . . ? N6 C71 C72 179.3(4) . . ? N7 C73 C74 178.5(4) . . ? N8 C75 C76 178.3(4) . . ? N9 C77 N9' 38.4(5) . . ? N9 C77 C78 164.0(6) . . ? N9' C77 C78 157.6(7) . . ? N10 C79 N10' 29.5(7) . . ? N10 C79 C80 170.2(9) . . ? N10' C79 C80 159.3(10) . . ? C12 N1 C9 125.9(2) . . ? C5 N2 C4 126.42(19) . . ? C51 N3 C47 112.2(2) . . ? C51 N3 C59 106.0(2) . . ? C47 N3 C59 111.3(2) . . ? C51 N3 C55 111.0(2) . . ? C47 N3 C55 105.30(19) . . ? C59 N3 C55 111.3(2) . . ? C31 N4 C35 110.7(2) . . ? C31 N4 C43 107.0(2) . . ? C35 N4 C43 111.0(2) . . ? C31 N4 C39 110.6(2) . . ? C35 N4 C39 107.4(2) . . ? C43 N4 C39 110.2(2) . . ? C15 N5 C27 111.0(2) . . ? C15 N5 C19 111.1(2) . . ? C27 N5 C19 106.88(19) . . ? C15 N5 C23 107.03(19) . . ? C27 N5 C23 110.5(2) . . ? C19 N5 C23 110.3(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.76 _refine_diff_density_min -0.84 _refine_diff_density_rms 0.07 data_mh252a _database_code_depnum_ccdc_archive 'CCDC 909164' #TrackingRef 'MnMo6-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H153 Mn Mo6 N8 O29' _chemical_formula_weight 2309.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 18.0293(7) _cell_length_b 20.8575(8) _cell_length_c 26.7597(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10062.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4509 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 19.8 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4768 _exptl_absorpt_coefficient_mu 0.919 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8669 _exptl_absorpt_correction_T_max 0.9642 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ApexII Quasar CCD' _diffrn_measurement_method '\w & \p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 69503 _diffrn_reflns_av_R_equivalents 0.1339 _diffrn_reflns_av_sigmaI/netI 0.1371 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 24.82 _reflns_number_total 16825 _reflns_number_gt 9760 _reflns_threshold_expression >2\s(I) _computing_data_collection Apex2 _computing_cell_refinement Apex2 _computing_data_reduction Apex2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics diamond3 _computing_publication_material WinGX _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^ > 2\s(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^)+(0.0736P)^2^+80.2740P] 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 SHELXL _refine_ls_extinction_coef 0.00113(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.47(7) _refine_ls_number_reflns 16825 _refine_ls_number_parameters 827 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1592 _refine_ls_R_factor_gt 0.0823 _refine_ls_wR_factor_ref 0.2247 _refine_ls_wR_factor_gt 0.1817 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.003 _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 0.60243(4) 0.82937(4) 0.22637(3) 0.0383(2) Uani 0.9124(6) 1 d P A 1 Mo2 Mo 0.62779(5) 0.66886(4) 0.21732(3) 0.0420(2) Uani 0.9124(6) 1 d P A 1 Mo3 Mo 0.74405(4) 0.59317(3) 0.29483(4) 0.0388(2) Uani 0.9124(6) 1 d P A 1 Mo4 Mo 0.83757(4) 0.67729(3) 0.38087(3) 0.0374(2) Uani 0.9124(6) 1 d P A 1 Mo5 Mo 0.80965(4) 0.83589(3) 0.39190(3) 0.0376(2) Uani 0.9124(6) 1 d P A 1 Mo6 Mo 0.69898(4) 0.91325(3) 0.31046(3) 0.0370(2) Uani 0.9124(6) 1 d P A 1 Mn1 Mn 0.71964(7) 0.75317(5) 0.30342(6) 0.0322(3) Uani 1 1 d . A 1 O1 O 0.6053(3) 0.8788(3) 0.2868(2) 0.0514(18) Uani 1 1 d . A 1 O2 O 0.7246(3) 0.8251(3) 0.2580(2) 0.0436(18) Uani 1 1 d . A 1 O3 O 0.6135(3) 0.7420(2) 0.2852(2) 0.0399(16) Uani 1 1 d . A 1 O4 O 0.6260(4) 0.8848(3) 0.1823(3) 0.059(2) Uani 1 1 d . A 1 O5 O 0.5064(3) 0.8214(3) 0.2217(3) 0.076(2) Uani 1 1 d . A 1 O6 O 0.6410(3) 0.7545(3) 0.1911(2) 0.0499(19) Uani 1 1 d . A 1 O7 O 0.5305(3) 0.6594(3) 0.2136(3) 0.065(2) Uani 1 1 d . A 1 O8 O 0.6646(4) 0.6255(3) 0.1678(3) 0.073(2) Uani 1 1 d . A 1 O9 O 0.6439(3) 0.6134(3) 0.2714(2) 0.0520(19) Uani 1 1 d . A 1 O10 O 0.7444(3) 0.6914(3) 0.2502(2) 0.0484(19) Uani 1 1 d . A 1 O11 O 0.7793(3) 0.5478(3) 0.2458(3) 0.058(2) Uani 1 1 d . A 1 O12 O 0.7233(4) 0.5383(3) 0.3375(2) 0.058(2) Uani 1 1 d . A 1 O13 O 0.8380(3) 0.6281(2) 0.3191(2) 0.0457(18) Uani 1 1 d . A 1 O14 O 0.7168(3) 0.6778(2) 0.3503(2) 0.0435(18) Uani 1 1 d . A 1 O15 O 0.9299(3) 0.6894(3) 0.3831(2) 0.0415(14) Uiso 1 1 d . A 1 O16 O 0.7991(3) 0.7509(2) 0.4163(2) 0.0439(18) Uani 1 1 d . A 1 O17 O 0.8212(3) 0.7630(2) 0.3238(2) 0.0357(16) Uani 1 1 d . A 1 O18 O 0.6912(3) 0.8152(2) 0.3588(2) 0.0407(17) Uani 1 1 d . A 1 O19 O 0.7928(3) 0.8922(3) 0.3346(2) 0.0468(18) Uani 1 1 d . A 1 O20 O 0.9007(3) 0.8463(3) 0.3957(3) 0.0536(19) Uani 1 1 d . A 1 O21 O 0.7743(4) 0.8772(3) 0.4411(2) 0.062(2) Uani 1 1 d . A 1 O22 O 0.6668(3) 0.9621(3) 0.3560(3) 0.055(2) Uani 1 1 d . A 1 O23 O 0.7244(4) 0.9638(3) 0.2629(3) 0.059(2) Uani 1 1 d . A 1 O24 O 0.8182(4) 0.6228(3) 0.4232(2) 0.058(2) Uani 1 1 d . A 1 O25 O 0.4635(4) 0.7959(3) 0.4028(3) 0.088(3) Uani 1 1 d . A 1 O26 O 0.9866(4) 0.7085(3) 0.2198(3) 0.084(3) Uani 1 1 d . A 1 O27 O 0.5980(6) 0.5870(5) 0.4683(4) 0.096(3) Uiso 0.80 1 d P B 1 O28 O 0.8612(5) 0.9033(4) 0.1312(3) 0.072(3) Uiso 0.80 1 d P C 1 O29 O 0.3968(6) 0.7876(5) 0.9615(4) 0.099(3) Uiso 0.80 1 d P D 1 N1 N 0.5406(4) 0.7150(3) 0.4135(3) 0.047(2) Uani 1 1 d . A 1 H1 H 0.5479 0.6808 0.4308 0.056 Uiso 1 1 calc R A 1 N2 N 0.9012(4) 0.7851(3) 0.1965(3) 0.048(2) Uani 1 1 d . A 1 H2 H 0.8935 0.8154 0.1754 0.057 Uiso 1 1 calc R A 1 N3 N 0.9203(4) 0.0388(3) 0.3487(3) 0.059(3) Uani 1 1 d . E 1 N4 N 0.0193(4) 0.5365(3) 0.2644(3) 0.093(4) Uani 1 1 d D F 1 N5 N 0.5728(4) 0.7455(4) 0.0531(3) 0.087(4) Uani 1 1 d D G 1 N6 N 0.7055(7) 0.5207(8) 0.4822(6) 0.077(5) Uiso 0.50 1 d PD B 1 N7 N 0.8241(5) 1.0057(4) 0.1376(5) 0.094(4) Uiso 0.80 1 d PD C 1 N8 N 0.3972(4) 0.8104(5) 0.8792(3) 0.070(3) Uiso 0.80 1 d PD D 1 C1 C 0.5996(4) 0.7309(4) 0.3760(3) 0.040(3) Uani 1 1 d . A 1 C2 C 0.6545(5) 0.6748(4) 0.3829(3) 0.055(3) Uani 1 1 d . A 1 H2A H 0.6720 0.6747 0.4172 0.066 Uiso 1 1 calc R A 1 H2B H 0.6284 0.6348 0.3772 0.066 Uiso 1 1 calc R A 1 C3 C 0.6335(4) 0.7969(4) 0.3892(4) 0.047(3) Uani 1 1 d . A 1 H3A H 0.5948 0.8291 0.3871 0.057 Uiso 1 1 calc R A 1 H3B H 0.6509 0.7958 0.4234 0.057 Uiso 1 1 calc R A 1 C4 C 0.5629(4) 0.7317(4) 0.3250(4) 0.053(3) Uani 1 1 d . A 1 H4A H 0.5379 0.6911 0.3198 0.063 Uiso 1 1 calc R A 1 H4B H 0.5257 0.7652 0.3245 0.063 Uiso 1 1 calc R A 1 C5 C 0.4780(5) 0.7470(4) 0.4237(4) 0.052(3) Uani 1 1 d . A 1 C6 C 0.4236(3) 0.7180(2) 0.4607(2) 0.048(3) Uani 1 1 d G A 1 C7 C 0.4447(4) 0.6754(3) 0.4981(2) 0.079(4) Uani 1 1 d G A 1 H7 H 0.4940 0.6628 0.5009 0.094 Uiso 1 1 calc R A 1 C8 C 0.3921(5) 0.6518(3) 0.5313(2) 0.109(5) Uani 1 1 d G A 1 H8 H 0.4061 0.6233 0.5563 0.131 Uiso 1 1 calc R A 1 C9 C 0.3184(4) 0.6706(4) 0.5271(3) 0.086(4) Uani 1 1 d G A 1 H9 H 0.2832 0.6548 0.5493 0.104 Uiso 1 1 calc R A 1 C10 C 0.2973(3) 0.7132(4) 0.4897(3) 0.092(5) Uani 1 1 d G A 1 H10 H 0.2480 0.7258 0.4869 0.110 Uiso 1 1 calc R A 1 C11 C 0.3499(3) 0.7368(3) 0.4565(2) 0.075(4) Uani 1 1 d G A 1 H11 H 0.3358 0.7653 0.4315 0.090 Uiso 1 1 calc R A 1 C12 C 0.8432(5) 0.7723(4) 0.2310(3) 0.044(3) Uani 1 1 d . A 1 C13 C 0.8759(5) 0.7732(4) 0.2854(3) 0.044(2) Uiso 1 1 d . A 1 H13A H 0.9136 0.7402 0.2880 0.053 Uiso 1 1 calc R A 1 H13B H 0.8998 0.8142 0.2910 0.053 Uiso 1 1 calc R A 1 C14 C 0.8083(5) 0.7055(4) 0.2186(4) 0.050(3) Uani 1 1 d . A 1 H14A H 0.7930 0.7048 0.1838 0.060 Uiso 1 1 calc R A 1 H14B H 0.8455 0.6724 0.2232 0.060 Uiso 1 1 calc R A 1 C15 C 0.7856(4) 0.8249(4) 0.2234(3) 0.038(2) Uiso 1 1 d . A 1 H15A H 0.8105 0.8660 0.2255 0.045 Uiso 1 1 calc R A 1 H15B H 0.7658 0.8210 0.1899 0.045 Uiso 1 1 calc R A 1 C16 C 0.9669(6) 0.7545(5) 0.1934(4) 0.066(4) Uani 1 1 d . A 1 C17 C 1.0231(3) 0.7761(3) 0.1549(2) 0.067(4) Uani 1 1 d G A 1 C18 C 1.0971(3) 0.7612(3) 0.1635(3) 0.088(4) Uani 1 1 d G A 1 H18 H 1.1106 0.7390 0.1922 0.106 Uiso 1 1 calc R A 1 C19 C 1.1510(3) 0.7795(4) 0.1292(3) 0.090(4) Uiso 1 1 d G A 1 H19 H 1.2005 0.7695 0.1349 0.108 Uiso 1 1 calc R A 1 C20 C 1.1308(5) 0.8127(5) 0.0862(3) 0.101(5) Uiso 1 1 d G A 1 H20 H 1.1668 0.8249 0.0633 0.122 Uiso 1 1 calc R A 1 C21 C 1.0568(5) 0.8276(4) 0.0776(3) 0.104(5) Uiso 1 1 d G A 1 H21 H 1.0433 0.8498 0.0489 0.124 Uiso 1 1 calc R A 1 C22 C 1.0029(4) 0.8093(3) 0.1119(3) 0.088(4) Uiso 1 1 d G A 1 H22 H 0.9533 0.8193 0.1062 0.105 Uiso 1 1 calc R A 1 C23 C 0.8585(5) 0.0232(5) 0.3830(4) 0.062(3) Uiso 1 1 d . E 1 H23A H 0.8703 -0.0176 0.3984 0.074 Uiso 1 1 calc R E 1 H23B H 0.8149 0.0163 0.3624 0.074 Uiso 1 1 calc R E 1 C24 C 0.8360(6) 0.0685(5) 0.4247(4) 0.063(3) Uiso 1 1 d . E 1 H24A H 0.8741 0.0686 0.4503 0.076 Uiso 1 1 calc R E 1 H24B H 0.8317 0.1117 0.4116 0.076 Uiso 1 1 calc R E 1 C25 C 0.7629(7) 0.0485(5) 0.4475(4) 0.102(4) Uani 1 1 d . E 1 H25A H 0.7660 0.0042 0.4583 0.123 Uiso 1 1 calc R E 1 H25B H 0.7241 0.0514 0.4224 0.123 Uiso 1 1 calc R E 1 C26 C 0.7430(6) 0.0913(6) 0.4922(5) 0.106(5) Uani 1 1 d . E 1 H26A H 0.7835 0.0915 0.5156 0.158 Uiso 1 1 calc R E 1 H26B H 0.6994 0.0749 0.5083 0.158 Uiso 1 1 calc R E 1 H26C H 0.7339 0.1342 0.4808 0.158 Uiso 1 1 calc R E 1 C27 C 0.9914(5) 0.0469(5) 0.3814(5) 0.077(4) Uani 1 1 d . E 1 H27A H 1.0340 0.0523 0.3596 0.092 Uiso 1 1 calc R E 1 H27B H 0.9866 0.0856 0.4013 0.092 Uiso 1 1 calc R E 1 C28 C 1.0053(6) -0.0083(7) 0.4153(4) 0.075(4) Uiso 0.80 1 d PD E 1 H28A H 1.0164 -0.0459 0.3954 0.090 Uiso 1 1 calc R E 1 H28B H 0.9606 -0.0171 0.4343 0.090 Uiso 1 1 calc R E 1 C29 C 1.0679(7) 0.0036(6) 0.4507(4) 0.077(5) Uiso 0.70 1 d PD E 1 H29A H 1.0754 -0.0347 0.4706 0.092 Uiso 0.70 1 calc PR E 1 H29B H 1.1127 0.0107 0.4314 0.092 Uiso 0.70 1 calc PR E 1 C30 C 1.0573(10) 0.0592(6) 0.4852(6) 0.092(6) Uiso 0.70 1 d PD E 1 H30A H 1.0594 0.0984 0.4665 0.138 Uiso 0.70 1 calc PR E 1 H30B H 1.0959 0.0591 0.5099 0.138 Uiso 0.70 1 calc PR E 1 H30C H 1.0100 0.0557 0.5014 0.138 Uiso 0.70 1 calc PR E 1 C31 C 0.9305(6) -0.0150(4) 0.3119(4) 0.074(3) Uani 1 1 d . E 1 H31A H 0.9351 -0.0550 0.3302 0.089 Uiso 1 1 calc R E 1 H31B H 0.8867 -0.0180 0.2911 0.089 Uiso 1 1 calc R E 1 C32 C 0.9954(6) -0.0071(4) 0.2800(4) 0.077(4) Uani 1 1 d . E 1 H32A H 1.0403 -0.0118 0.2997 0.093 Uiso 1 1 calc R E 1 H32B H 0.9954 0.0355 0.2654 0.093 Uiso 1 1 calc R E 1 C33 C 0.9933(7) -0.0576(5) 0.2390(5) 0.106(5) Uani 1 1 d . E 1 H33A H 0.9508 -0.0499 0.2176 0.127 Uiso 1 1 calc R E 1 H33B H 0.9877 -0.0997 0.2539 0.127 Uiso 1 1 calc R E 1 C34 C 1.0656(7) -0.0561(5) 0.2069(5) 0.107(5) Uani 1 1 d . E 1 H34A H 1.0702 -0.0150 0.1910 0.160 Uiso 1 1 calc R E 1 H34B H 1.0632 -0.0890 0.1818 0.160 Uiso 1 1 calc R E 1 H34C H 1.1078 -0.0634 0.2280 0.160 Uiso 1 1 calc R E 1 C35 C 0.9101(6) 0.1044(5) 0.3235(4) 0.076(4) Uani 1 1 d . E 1 H35A H 0.8986 0.1355 0.3493 0.091 Uiso 1 1 calc R E 1 H35B H 0.9572 0.1168 0.3089 0.091 Uiso 1 1 calc R E 1 C36 C 0.8508(6) 0.1095(7) 0.2831(7) 0.139(7) Uani 1 1 d . E 1 H36A H 0.8055 0.0878 0.2928 0.167 Uiso 1 1 calc R E 1 H36B H 0.8681 0.0923 0.2515 0.167 Uiso 1 1 calc R E 1 C37 C 0.8387(9) 0.1895(7) 0.2801(6) 0.128(6) Uiso 1 1 d . E 1 H37A H 0.8296 0.2071 0.3131 0.154 Uiso 1 1 calc R E 1 H37B H 0.8822 0.2101 0.2661 0.154 Uiso 1 1 calc R E 1 C38 C 0.7691(12) 0.2003(11) 0.2452(8) 0.150(8) Uiso 0.80 1 d P E 1 H38A H 0.7829 0.1929 0.2110 0.225 Uiso 0.80 1 calc PR E 1 H38B H 0.7516 0.2436 0.2488 0.225 Uiso 0.80 1 calc PR E 1 H38C H 0.7304 0.1711 0.2545 0.225 Uiso 0.80 1 calc PR E 1 C39 C 0.0940(5) 0.5311(4) 0.2380(4) 0.073(3) Uiso 1 1 d D F 1 H39A H 0.1320 0.5254 0.2633 0.088 Uiso 1 1 calc R F 1 H39B H 0.0934 0.4926 0.2177 0.088 Uiso 1 1 calc R F 1 C40 C 0.1167(5) 0.5861(5) 0.2053(5) 0.117(5) Uiso 1 1 d D F 1 H40A H 0.0876 0.5856 0.1748 0.141 Uiso 1 1 calc R F 1 H40B H 0.1073 0.6263 0.2224 0.141 Uiso 1 1 calc R F 1 C41 C 0.1973(6) 0.5813(7) 0.1926(5) 0.093(6) Uiso 0.70 1 d PD F 1 H41A H 0.2190 0.6226 0.1845 0.111 Uiso 1 1 calc R F 1 H41B H 0.2258 0.5607 0.2188 0.111 Uiso 1 1 calc R F 1 C42 C 0.1885(9) 0.5400(7) 0.1482(5) 0.083(5) Uiso 0.70 1 d PD F 1 H42A H 0.1689 0.4991 0.1581 0.124 Uiso 0.70 1 calc PR F 1 H42B H 0.2358 0.5341 0.1324 0.124 Uiso 0.70 1 calc PR F 1 H42C H 0.1549 0.5600 0.1251 0.124 Uiso 0.70 1 calc PR F 1 C43 C -0.0384(5) 0.5574(5) 0.2282(3) 0.077(3) Uiso 1 1 d D F 1 H43A H -0.0208 0.5963 0.2121 0.093 Uiso 1 1 calc R F 1 H43B H -0.0824 0.5688 0.2470 0.093 Uiso 1 1 calc R F 1 C44 C -0.0616(7) 0.5107(5) 0.1872(4) 0.109(5) Uiso 1 1 d D F 1 H44A H -0.0912 0.4768 0.2020 0.131 Uiso 1 1 calc R F 1 H44B H -0.0175 0.4912 0.1730 0.131 Uiso 1 1 calc R F 1 C45 C -0.1060(7) 0.5426(6) 0.1455(4) 0.130(6) Uiso 1 1 d D F 1 H45A H -0.1226 0.5099 0.1222 0.156 Uiso 1 1 calc R F 1 H45B H -0.1497 0.5627 0.1597 0.156 Uiso 1 1 calc R F 1 C46 C -0.0620(11) 0.5922(8) 0.1175(8) 0.121(9) Uiso 0.60 1 d PD F 1 H46A H -0.0459 0.6249 0.1403 0.182 Uiso 0.60 1 calc PR F 1 H46B H -0.0924 0.6110 0.0920 0.182 Uiso 0.60 1 calc PR F 1 H46C H -0.0195 0.5723 0.1024 0.182 Uiso 0.60 1 calc PR F 1 C47 C -0.0030(5) 0.4746(5) 0.2903(4) 0.095(4) Uiso 1 1 d D F 1 H47A H -0.0069 0.4415 0.2649 0.114 Uiso 1 1 calc R F 1 H47B H 0.0370 0.4623 0.3125 0.114 Uiso 1 1 calc R F 1 C48 C -0.0738(6) 0.4741(5) 0.3200(5) 0.115(5) Uiso 1 1 d D F 1 H48A H -0.1152 0.4832 0.2980 0.138 Uiso 1 1 calc R F 1 H48B H -0.0717 0.5075 0.3452 0.138 Uiso 1 1 calc R F 1 C49 C -0.0860(6) 0.4104(6) 0.3450(6) 0.123(7) Uiso 0.80 1 d PD F 1 H49A H -0.0727 0.3768 0.3217 0.148 Uiso 0.80 1 calc PR F 1 H49B H -0.0526 0.4073 0.3733 0.148 Uiso 0.80 1 calc PR F 1 C50 C -0.1635(8) 0.3982(19) 0.3631(13) 0.156(17) Uiso 0.40 1 d PD F 1 H50A H -0.1956 0.3914 0.3350 0.234 Uiso 0.40 1 calc PR F 1 H50B H -0.1806 0.4346 0.3818 0.234 Uiso 0.40 1 calc PR F 1 H50C H -0.1639 0.3609 0.3841 0.234 Uiso 0.40 1 calc PR F 1 C50' C -0.1198(12) 0.3573(10) 0.3076(9) 0.069(6) Uiso 0.50 1 d P H 2 C51 C 0.0269(6) 0.5899(5) 0.3032(3) 0.082(3) Uiso 1 1 d D . . H51A H 0.0447 0.6281 0.2864 0.099 Uiso 1 1 calc R F 1 H51B H -0.0220 0.5995 0.3163 0.099 Uiso 1 1 calc R F 1 C52 C 0.0781(7) 0.5758(6) 0.3468(5) 0.087(5) Uiso 0.70 1 d PD F . H52A H 0.0502 0.5534 0.3724 0.105 Uiso 0.70 1 calc PR . . H52B H 0.1171 0.5473 0.3355 0.105 Uiso 0.70 1 calc PR . . C53 C 0.1134(7) 0.6346(7) 0.3700(5) 0.136(7) Uiso 0.80 1 d PD . . H53A H 0.1360 0.6582 0.3427 0.163 Uiso 0.80 1 calc PR F . H53B H 0.0730 0.6608 0.3823 0.163 Uiso 0.80 1 calc PR . . C54 C 0.1697(12) 0.632(3) 0.4107(8) 0.077(17) Uiso 0.20 1 d PD F . H54A H 0.1659 0.5922 0.4281 0.116 Uiso 0.20 1 calc PR . . H54B H 0.1610 0.6669 0.4336 0.116 Uiso 0.20 1 calc PR . . H54C H 0.2184 0.6364 0.3966 0.116 Uiso 0.20 1 calc PR . . C55 C 0.6483(5) 0.7342(7) 0.0759(4) 0.107(5) Uiso 1 1 d D . . H55A H 0.6556 0.7653 0.1024 0.128 Uiso 1 1 calc R G 1 H55B H 0.6485 0.6920 0.0911 0.128 Uiso 1 1 calc R G 1 C56 C 0.7130(5) 0.7385(7) 0.0407(5) 0.122(5) Uiso 1 1 d D G . H56A H 0.7123 0.7797 0.0239 0.146 Uiso 1 1 calc R . . H56B H 0.7088 0.7053 0.0155 0.146 Uiso 1 1 calc R . . C57 C 0.7856(5) 0.7308(7) 0.0682(4) 0.100(4) Uiso 1 1 d D . . H57A H 0.7883 0.7636 0.0939 0.120 Uiso 1 1 calc R G . H57B H 0.7854 0.6895 0.0849 0.120 Uiso 1 1 calc R . . C58 C 0.8537(7) 0.7351(8) 0.0369(6) 0.083(5) Uiso 0.70 1 d PD G . H58A H 0.8460 0.7121 0.0062 0.125 Uiso 0.70 1 calc PR . . H58B H 0.8948 0.7166 0.0546 0.125 Uiso 0.70 1 calc PR . . H58C H 0.8642 0.7793 0.0296 0.125 Uiso 0.70 1 calc PR . . C59 C 0.5569(8) 0.6953(4) 0.0146(4) 0.109(5) Uiso 1 1 d D . . H59A H 0.5914 0.7004 -0.0129 0.130 Uiso 1 1 calc R G 1 H59B H 0.5073 0.7019 0.0016 0.130 Uiso 1 1 calc R G 1 C60 C 0.5629(8) 0.6266(4) 0.0348(5) 0.077(5) Uiso 0.70 1 d PD G . H60A H 0.6143 0.6173 0.0426 0.092 Uiso 0.70 1 calc PR . . H60B H 0.5346 0.6233 0.0656 0.092 Uiso 0.70 1 calc PR . . C61 C 0.5347(10) 0.5783(5) -0.0019(6) 0.087(6) Uiso 0.60 1 d PD . . H61A H 0.4823 0.5867 -0.0066 0.105 Uiso 1 1 calc R G . H61B H 0.5587 0.5873 -0.0336 0.105 Uiso 1 1 calc R . . C62 C 0.5428(15) 0.5085(6) 0.0074(10) 0.110(10) Uiso 0.50 1 d PD G . H62A H 0.5624 0.4881 -0.0219 0.164 Uiso 0.50 1 calc PR . . H62B H 0.4952 0.4905 0.0153 0.164 Uiso 0.50 1 calc PR . . H62C H 0.5760 0.5019 0.0350 0.164 Uiso 0.50 1 calc PR . . C63 C 0.5174(5) 0.7401(6) 0.0954(4) 0.089(4) Uiso 1 1 d D . . H63A H 0.5344 0.7672 0.1225 0.107 Uiso 1 1 calc R G 1 H63B H 0.5180 0.6962 0.1073 0.107 Uiso 1 1 calc R G 1 C64 C 0.4379(5) 0.7579(8) 0.0837(4) 0.116(6) Uiso 0.90 1 d PD G . H64A H 0.4358 0.8024 0.0733 0.140 Uiso 1 1 calc R . . H64B H 0.4201 0.7317 0.0563 0.140 Uiso 1 1 calc R . . C65 C 0.3890(8) 0.7486(5) 0.1277(5) 0.099(5) Uiso 0.80 1 d PD . . H65A H 0.4104 0.7714 0.1558 0.119 Uiso 0.80 1 calc PR G . H65B H 0.3413 0.7680 0.1206 0.119 Uiso 0.80 1 calc PR . . C66 C 0.3766(17) 0.6817(6) 0.1426(11) 0.135(12) Uiso 0.50 1 d PD G . H66A H 0.3445 0.6612 0.1189 0.202 Uiso 0.50 1 calc PR . . H66B H 0.3541 0.6805 0.1751 0.202 Uiso 0.50 1 calc PR . . H66C H 0.4233 0.6594 0.1436 0.202 Uiso 0.50 1 calc PR . . C67 C 0.5711(9) 0.8107(4) 0.0269(5) 0.137(6) Uiso 1 1 d D . . H67A H 0.6022 0.8093 -0.0026 0.165 Uiso 1 1 calc R G 1 H67B H 0.5208 0.8203 0.0164 0.165 Uiso 1 1 calc R G 1 C68 C 0.5981(9) 0.8624(5) 0.0612(5) 0.107(6) Uiso 0.80 1 d PD G . H68A H 0.5700 0.8628 0.0921 0.129 Uiso 0.80 1 calc PR . . H68B H 0.6503 0.8568 0.0689 0.129 Uiso 0.80 1 calc PR . . C69 C 0.5856(8) 0.9221(4) 0.0324(5) 0.091(5) Uiso 0.80 1 d PD . . H69A H 0.5330 0.9273 0.0258 0.109 Uiso 0.80 1 calc PR G . H69B H 0.6113 0.9195 0.0006 0.109 Uiso 0.80 1 calc PR . . C70 C 0.6137(11) 0.9787(7) 0.0614(7) 0.076(7) Uiso 0.50 1 d PD G . H70A H 0.5808 0.9872 0.0889 0.113 Uiso 0.50 1 calc PR . . H70B H 0.6158 1.0155 0.0400 0.113 Uiso 0.50 1 calc PR . . H70C H 0.6624 0.9695 0.0740 0.113 Uiso 0.50 1 calc PR . . C71 C 0.6474(7) 0.5508(7) 0.4558(6) 0.096(5) Uiso 0.80 1 d PD . . H71 H 0.6468 0.5410 0.4219 0.115 Uiso 0.80 1 calc PR B 1 C72 C 0.7463(12) 0.4832(10) 0.4578(8) 0.074(7) Uiso 0.50 1 d P . . H72A H 0.7167 0.4491 0.4443 0.111 Uiso 0.50 1 calc PR B 1 H72B H 0.7835 0.4657 0.4794 0.111 Uiso 0.50 1 calc PR B 1 H72C H 0.7696 0.5062 0.4310 0.111 Uiso 0.50 1 calc PR B 1 C73 C 0.721(3) 0.566(2) 0.5205(18) 0.055(13) Uiso 0.20 1 d P . . H73A H 0.7253 0.6079 0.5062 0.082 Uiso 0.20 1 calc PR B 1 H73B H 0.7669 0.5547 0.5366 0.082 Uiso 0.20 1 calc PR B 1 H73C H 0.6817 0.5655 0.5446 0.082 Uiso 0.20 1 calc PR B 1 C74 C 0.8077(9) 0.9407(5) 0.1415(6) 0.088(5) Uiso 0.80 1 d PD . . H74 H 0.7611 0.9258 0.1510 0.106 Uiso 0.80 1 calc PR C 1 C75 C 0.7618(7) 1.0464(7) 0.1518(7) 0.124(7) Uiso 0.80 1 d PD . . H75A H 0.7339 1.0577 0.1226 0.186 Uiso 0.80 1 calc PR C 1 H75B H 0.7801 1.0846 0.1675 0.186 Uiso 0.80 1 calc PR C 1 H75C H 0.7304 1.0236 0.1748 0.186 Uiso 0.80 1 calc PR C 1 C76 C 0.8992(6) 1.0287(8) 0.1252(7) 0.111(6) Uiso 0.80 1 d PD . . H76A H 0.9223 1.0457 0.1547 0.167 Uiso 0.80 1 calc PR C 1 H76B H 0.8960 1.0616 0.1002 0.167 Uiso 0.80 1 calc PR C 1 H76C H 0.9283 0.9937 0.1126 0.167 Uiso 0.80 1 calc PR C 1 C77 C 0.4270(8) 0.7905(7) 0.9263(4) 0.080(4) Uiso 0.80 1 d PD . . H77 H 0.4768 0.7789 0.9269 0.095 Uiso 0.80 1 calc PR D 1 C78 C 0.3174(6) 0.8283(10) 0.8771(10) 0.118(8) Uiso 0.60 1 d PD . . H78A H 0.3112 0.8646 0.8555 0.178 Uiso 0.60 1 calc PR D 1 H78B H 0.3004 0.8389 0.9101 0.178 Uiso 0.60 1 calc PR D 1 H78C H 0.2891 0.7928 0.8644 0.178 Uiso 0.60 1 calc PR D 1 C79 C 0.4412(8) 0.8165(8) 0.8313(4) 0.091(5) Uiso 0.80 1 d PD . . H79A H 0.4296 0.8565 0.8154 0.137 Uiso 0.80 1 calc PR D 1 H79B H 0.4288 0.7817 0.8094 0.137 Uiso 0.80 1 calc PR D 1 H79C H 0.4932 0.8151 0.8389 0.137 Uiso 0.80 1 calc PR D 1 Mo1' Mo 0.6343(6) 0.8161(5) 0.1958(4) 0.053(3) Uiso 0.0876(6) 1 d P A 2 Mo2' Mo 0.7220(6) 0.9064(5) 0.2790(4) 0.052(3) Uiso 0.0876(6) 1 d P A 2 Mo3' Mo 0.8338(7) 0.8348(6) 0.3629(5) 0.069(3) Uiso 0.0876(6) 1 d P A 2 Mo4' Mo 0.8632(7) 0.6777(6) 0.3553(5) 0.066(3) Uiso 0.0876(6) 1 d P A 2 Mo5' Mo 0.7720(7) 0.5868(6) 0.2703(5) 0.067(3) Uiso 0.0876(6) 1 d P A 2 Mo6' Mo 0.6586(7) 0.6560(6) 0.1892(5) 0.064(3) Uiso 0.0876(6) 1 d P A 2 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 0.0410(4) 0.0324(4) 0.0415(5) 0.0062(4) -0.0153(4) 0.0006(4) Mo2 0.0527(5) 0.0297(4) 0.0437(5) 0.0017(4) -0.0147(4) -0.0111(4) Mo3 0.0422(4) 0.0225(3) 0.0517(5) 0.0027(4) -0.0034(4) -0.0016(3) Mo4 0.0381(4) 0.0328(4) 0.0414(5) 0.0086(4) -0.0114(4) 0.0046(3) Mo5 0.0407(4) 0.0312(4) 0.0409(5) -0.0023(4) -0.0141(4) -0.0041(3) Mo6 0.0372(4) 0.0240(3) 0.0498(5) -0.0024(4) -0.0099(4) 0.0000(3) Mn1 0.0327(5) 0.0190(4) 0.0449(7) 0.0056(5) -0.0114(5) -0.0011(4) O1 0.061(3) 0.038(3) 0.055(4) 0.003(3) -0.012(3) -0.027(3) O2 0.054(3) 0.052(3) 0.025(3) 0.000(3) -0.010(3) -0.007(3) O3 0.032(3) 0.027(3) 0.060(4) 0.019(3) -0.027(3) -0.004(2) O4 0.068(4) 0.034(3) 0.074(5) 0.025(3) -0.009(4) -0.004(3) O5 0.047(3) 0.082(4) 0.099(5) 0.033(4) -0.040(4) -0.030(3) O6 0.057(4) 0.055(4) 0.038(4) 0.011(3) -0.019(3) -0.017(3) O7 0.054(3) 0.061(4) 0.079(5) 0.013(4) -0.022(4) -0.038(3) O8 0.115(6) 0.044(4) 0.061(5) -0.016(3) -0.017(4) 0.001(4) O9 0.050(3) 0.036(3) 0.070(4) 0.017(3) -0.022(3) 0.006(3) O10 0.056(4) 0.047(3) 0.042(4) 0.007(3) 0.005(3) -0.003(3) O11 0.058(4) 0.044(3) 0.073(5) -0.025(3) -0.004(4) 0.008(3) O12 0.069(4) 0.037(3) 0.070(5) 0.030(3) -0.001(4) 0.006(3) O13 0.038(3) 0.029(3) 0.070(4) 0.015(3) -0.012(3) 0.017(2) O14 0.030(3) 0.016(2) 0.085(5) 0.004(3) -0.009(3) -0.008(2) O16 0.049(3) 0.037(3) 0.046(4) -0.004(3) -0.019(3) -0.006(3) O17 0.040(3) 0.031(3) 0.036(3) -0.009(3) 0.010(3) 0.019(2) O18 0.022(3) 0.029(3) 0.071(4) 0.010(3) -0.025(3) -0.007(2) O19 0.060(4) 0.037(3) 0.043(4) -0.016(3) -0.003(3) -0.017(3) O20 0.039(3) 0.045(3) 0.077(5) -0.022(3) -0.022(3) 0.015(3) O21 0.072(4) 0.064(4) 0.049(4) 0.009(4) -0.003(4) -0.009(4) O22 0.039(3) 0.047(3) 0.078(5) -0.023(3) -0.013(3) -0.008(3) O23 0.063(4) 0.031(3) 0.083(5) 0.017(3) -0.024(4) -0.021(3) O24 0.072(4) 0.051(4) 0.051(4) 0.015(3) -0.012(4) 0.012(3) O25 0.042(4) 0.071(4) 0.150(8) 0.031(5) 0.003(4) 0.011(3) O26 0.070(4) 0.044(3) 0.136(7) 0.048(4) -0.005(5) 0.010(3) N1 0.045(4) 0.041(4) 0.054(5) 0.009(4) -0.012(4) -0.006(3) N2 0.062(5) 0.041(4) 0.040(5) 0.004(4) -0.003(4) -0.003(4) N3 0.057(5) 0.041(4) 0.079(6) -0.009(4) -0.021(4) -0.009(4) N4 0.074(6) 0.094(7) 0.112(8) 0.047(6) 0.032(6) 0.030(5) N5 0.068(6) 0.130(8) 0.064(6) -0.021(6) -0.012(5) 0.014(5) C1 0.033(4) 0.034(4) 0.053(6) 0.004(4) -0.012(4) 0.003(3) C2 0.097(7) 0.036(4) 0.031(5) 0.003(5) 0.007(5) -0.020(5) C3 0.037(4) 0.056(5) 0.049(6) -0.015(5) -0.015(5) 0.003(4) C4 0.031(4) 0.036(4) 0.091(8) -0.006(5) -0.029(5) -0.013(4) C5 0.040(5) 0.034(4) 0.082(7) 0.021(5) 0.002(5) 0.029(4) C6 0.043(5) 0.053(5) 0.048(6) 0.000(5) 0.013(5) -0.002(4) C7 0.103(9) 0.065(7) 0.068(8) 0.009(6) 0.014(7) 0.015(6) C8 0.085(9) 0.115(9) 0.127(10) 0.074(8) 0.022(8) -0.007(8) C9 0.110(9) 0.065(7) 0.084(8) -0.040(6) 0.015(7) 0.009(7) C10 0.111(9) 0.044(6) 0.121(11) 0.005(7) 0.000(9) -0.031(6) C11 0.061(7) 0.057(6) 0.108(10) -0.017(6) -0.004(7) 0.007(5) C12 0.050(5) 0.038(4) 0.045(6) -0.006(4) 0.011(5) -0.020(4) C14 0.077(6) 0.030(4) 0.042(6) 0.008(4) 0.013(5) 0.000(4) C16 0.053(6) 0.054(6) 0.090(8) -0.023(6) 0.012(6) -0.018(5) C17 0.081(7) 0.051(6) 0.070(8) -0.018(6) -0.006(6) 0.002(6) C18 0.075(7) 0.095(8) 0.094(9) -0.004(7) 0.026(7) -0.043(6) C25 0.114(9) 0.102(7) 0.091(8) -0.076(6) 0.038(7) -0.062(6) C26 0.066(7) 0.123(10) 0.128(10) -0.068(8) 0.026(8) -0.012(7) C27 0.043(5) 0.072(6) 0.115(9) -0.050(6) -0.011(6) -0.006(5) C31 0.097(7) 0.052(5) 0.072(7) -0.024(6) 0.008(7) -0.042(5) C32 0.091(7) 0.053(5) 0.088(8) -0.040(6) 0.025(6) -0.037(5) C33 0.148(10) 0.075(6) 0.096(9) -0.062(6) 0.013(8) -0.061(7) C34 0.150(11) 0.061(7) 0.110(10) -0.041(7) 0.072(8) -0.029(7) C35 0.095(8) 0.064(7) 0.069(7) -0.010(6) -0.042(6) -0.004(6) C36 0.029(6) 0.144(12) 0.244(19) -0.047(13) 0.001(9) -0.012(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O4 1.704(6) . ? Mo1 O5 1.744(6) . ? Mo1 O1 1.918(6) . ? Mo1 O6 1.953(6) . ? Mo1 O2 2.361(6) . ? Mo1 O3 2.416(5) . ? Mo2 O8 1.735(7) . ? Mo2 O7 1.768(6) . ? Mo2 O9 1.876(6) . ? Mo2 O6 1.934(6) . ? Mo2 O10 2.328(6) . ? Mo2 O3 2.388(6) . ? Mo3 O12 1.659(6) . ? Mo3 O11 1.738(6) . ? Mo3 O13 1.955(5) . ? Mo3 O9 1.957(6) . ? Mo3 O14 2.357(6) . ? Mo3 O10 2.372(6) . ? Mo4 O24 1.642(6) . ? Mo4 O15 1.685(5) . ? Mo4 O16 1.934(6) . ? Mo4 O13 1.944(6) . ? Mo4 O14 2.326(5) . ? Mo4 O17 2.371(5) . ? Mo5 O20 1.658(5) . ? Mo5 O21 1.698(7) . ? Mo5 O16 1.898(5) . ? Mo5 O19 1.955(6) . ? Mo5 O18 2.351(5) . ? Mo5 O17 2.382(5) . ? Mo6 O22 1.690(6) . ? Mo6 O23 1.714(6) . ? Mo6 O19 1.864(6) . ? Mo6 O1 1.943(6) . ? Mo6 O2 2.360(6) . ? Mo6 O18 2.424(5) . ? Mn1 O17 1.921(5) . ? Mn1 O2 1.933(6) . ? Mn1 O10 1.973(6) . ? Mn1 O3 1.989(5) . ? Mn1 O14 2.012(6) . ? Mn1 O18 2.033(6) . ? O2 C15 1.436(10) . ? O3 C4 1.418(11) . ? O10 C14 1.458(11) . ? O14 C2 1.424(11) . ? O17 C13 1.440(10) . ? O18 C3 1.374(10) . ? O25 C5 1.192(11) . ? O26 C16 1.244(12) . ? O27 C71 1.215(17) . ? O28 C74 1.271(16) . ? O29 C77 1.089(16) . ? N1 C5 1.338(11) . ? N1 C1 1.499(11) . ? N2 C16 1.348(12) . ? N2 C12 1.419(11) . ? N3 C23 1.479(12) . ? N3 C31 1.504(12) . ? N3 C35 1.535(13) . ? N3 C27 1.562(12) . ? N4 C43 1.488(10) . ? N4 C47 1.519(11) . ? N4 C39 1.525(10) . ? N4 C51 1.528(11) . ? N5 C59 1.497(11) . ? N5 C55 1.509(11) . ? N5 C63 1.513(11) . ? N5 C67 1.531(11) . ? N6 C72 1.26(3) . ? N6 C71 1.411(14) . ? N6 C73 1.42(5) . ? N7 C74 1.391(12) . ? N7 C75 1.459(13) . ? N7 C76 1.475(13) . ? N8 C77 1.433(12) . ? N8 C78 1.486(13) . ? N8 C79 1.512(12) . ? C1 C4 1.517(13) . ? C1 C2 1.542(12) . ? C1 C3 1.547(11) . ? C5 C6 1.520(11) . ? C6 C7 1.3900 . ? C6 C11 1.3900 . ? C7 C8 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C12 C15 1.524(11) . ? C12 C14 1.564(11) . ? C12 C13 1.571(12) . ? C16 C17 1.514(12) . ? C17 C18 1.3900 . ? C17 C22 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C23 C24 1.518(14) . ? C24 C25 1.511(15) . ? C25 C26 1.536(16) . ? C27 C28 1.486(16) . ? C28 C29 1.496(13) . ? C29 C30 1.493(14) . ? C31 C32 1.458(15) . ? C32 C33 1.522(14) . ? C33 C34 1.562(17) . ? C35 C36 1.523(18) . ? C36 C37 1.68(2) . ? C37 C38 1.58(3) . ? C39 C40 1.500(12) . ? C40 C41 1.495(12) . ? C41 C42 1.477(14) . ? C43 C44 1.524(12) . ? C44 C45 1.527(13) . ? C45 C46 1.504(15) . ? C47 C48 1.503(12) . ? C48 C49 1.504(13) . ? C49 C50 1.500(16) . ? C51 C52 1.517(13) . ? C52 C53 1.514(14) . ? C53 C54 1.490(17) . ? C55 C56 1.503(12) . ? C56 C57 1.510(12) . ? C57 C58 1.490(13) . ? C59 C60 1.535(12) . ? C60 C61 1.498(14) . ? C61 C62 1.484(14) . ? C63 C64 1.514(12) . ? C64 C65 1.484(13) . ? C65 C66 1.470(15) . ? C67 C68 1.497(13) . ? C68 C69 1.481(13) . ? C69 C70 1.500(15) . ? 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 Mo1 O5 105.2(3) . . ? O4 Mo1 O1 102.2(3) . . ? O5 Mo1 O1 98.0(3) . . ? O4 Mo1 O6 96.8(3) . . ? O5 Mo1 O6 104.0(3) . . ? O1 Mo1 O6 145.9(2) . . ? O4 Mo1 O2 92.3(3) . . ? O5 Mo1 O2 161.5(3) . . ? O1 Mo1 O2 72.2(2) . . ? O6 Mo1 O2 79.1(2) . . ? O4 Mo1 O3 160.3(3) . . ? O5 Mo1 O3 93.2(3) . . ? O1 Mo1 O3 81.6(2) . . ? O6 Mo1 O3 71.5(2) . . ? O2 Mo1 O3 70.20(18) . . ? O8 Mo2 O7 106.2(3) . . ? O8 Mo2 O9 102.0(3) . . ? O7 Mo2 O9 97.4(3) . . ? O8 Mo2 O6 99.0(3) . . ? O7 Mo2 O6 101.8(3) . . ? O9 Mo2 O6 146.2(3) . . ? O8 Mo2 O10 92.7(3) . . ? O7 Mo2 O10 160.1(3) . . ? O9 Mo2 O10 72.1(2) . . ? O6 Mo2 O10 80.7(2) . . ? O8 Mo2 O3 162.8(3) . . ? O7 Mo2 O3 90.4(3) . . ? O9 Mo2 O3 79.8(2) . . ? O6 Mo2 O3 72.5(2) . . ? O10 Mo2 O3 71.41(19) . . ? O12 Mo3 O11 103.1(3) . . ? O12 Mo3 O13 102.9(3) . . ? O11 Mo3 O13 97.9(3) . . ? O12 Mo3 O9 99.2(3) . . ? O11 Mo3 O9 102.3(3) . . ? O13 Mo3 O9 145.6(2) . . ? O12 Mo3 O14 92.1(3) . . ? O11 Mo3 O14 163.5(2) . . ? O13 Mo3 O14 72.1(2) . . ? O9 Mo3 O14 81.2(2) . . ? O12 Mo3 O10 160.6(3) . . ? O11 Mo3 O10 95.1(3) . . ? O13 Mo3 O10 81.0(2) . . ? O9 Mo3 O10 69.8(2) . . ? O14 Mo3 O10 70.8(2) . . ? O24 Mo4 O15 106.8(3) . . ? O24 Mo4 O16 97.8(3) . . ? O15 Mo4 O16 102.5(3) . . ? O24 Mo4 O13 102.8(3) . . ? O15 Mo4 O13 96.1(3) . . ? O16 Mo4 O13 146.9(2) . . ? O24 Mo4 O14 92.7(3) . . ? O15 Mo4 O14 159.5(3) . . ? O16 Mo4 O14 80.4(2) . . ? O13 Mo4 O14 73.0(2) . . ? O24 Mo4 O17 160.1(3) . . ? O15 Mo4 O17 91.9(2) . . ? O16 Mo4 O17 70.9(2) . . ? O13 Mo4 O17 81.4(2) . . ? O14 Mo4 O17 69.72(18) . . ? O20 Mo5 O21 105.0(3) . . ? O20 Mo5 O16 101.5(3) . . ? O21 Mo5 O16 99.7(3) . . ? O20 Mo5 O19 97.0(3) . . ? O21 Mo5 O19 104.2(3) . . ? O16 Mo5 O19 144.6(2) . . ? O20 Mo5 O18 161.0(3) . . ? O21 Mo5 O18 92.5(3) . . ? O16 Mo5 O18 82.4(2) . . ? O19 Mo5 O18 71.0(2) . . ? O20 Mo5 O17 92.5(3) . . ? O21 Mo5 O17 161.8(3) . . ? O16 Mo5 O17 71.2(2) . . ? O19 Mo5 O17 78.3(2) . . ? O18 Mo5 O17 70.97(19) . . ? O22 Mo6 O23 104.8(3) . . ? O22 Mo6 O19 101.7(3) . . ? O23 Mo6 O19 99.2(3) . . ? O22 Mo6 O1 99.2(3) . . ? O23 Mo6 O1 102.6(3) . . ? O19 Mo6 O1 144.7(2) . . ? O22 Mo6 O2 165.0(2) . . ? O23 Mo6 O2 89.1(2) . . ? O19 Mo6 O2 81.1(2) . . ? O1 Mo6 O2 71.8(2) . . ? O22 Mo6 O18 96.0(3) . . ? O23 Mo6 O18 158.4(3) . . ? O19 Mo6 O18 70.6(2) . . ? O1 Mo6 O18 79.2(2) . . ? O2 Mo6 O18 70.83(19) . . ? O17 Mn1 O2 92.9(2) . . ? O17 Mn1 O10 93.4(2) . . ? O2 Mn1 O10 92.4(2) . . ? O17 Mn1 O3 177.6(3) . . ? O2 Mn1 O3 88.9(2) . . ? O10 Mn1 O3 88.0(2) . . ? O17 Mn1 O14 86.1(2) . . ? O2 Mn1 O14 178.7(3) . . ? O10 Mn1 O14 86.9(2) . . ? O3 Mn1 O14 92.1(2) . . ? O17 Mn1 O18 88.0(2) . . ? O2 Mn1 O18 88.7(2) . . ? O10 Mn1 O18 178.2(2) . . ? O3 Mn1 O18 90.6(2) . . ? O14 Mn1 O18 92.1(2) . . ? Mo1 O1 Mo6 119.8(3) . . ? C15 O2 Mn1 116.0(5) . . ? C15 O2 Mo6 122.4(5) . . ? Mn1 O2 Mo6 102.8(2) . . ? C15 O2 Mo1 118.9(5) . . ? Mn1 O2 Mo1 102.2(2) . . ? Mo6 O2 Mo1 90.0(2) . . ? C4 O3 Mn1 116.9(5) . . ? C4 O3 Mo2 122.9(4) . . ? Mn1 O3 Mo2 99.0(2) . . ? C4 O3 Mo1 123.5(4) . . ? Mn1 O3 Mo1 98.7(2) . . ? Mo2 O3 Mo1 89.7(2) . . ? Mo2 O6 Mo1 121.2(3) . . ? Mo2 O9 Mo3 121.5(3) . . ? C14 O10 Mn1 117.8(5) . . ? C14 O10 Mo2 122.4(5) . . ? Mn1 O10 Mo2 101.5(3) . . ? C14 O10 Mo3 117.9(5) . . ? Mn1 O10 Mo3 101.5(2) . . ? Mo2 O10 Mo3 90.7(2) . . ? Mo4 O13 Mo3 118.4(3) . . ? C2 O14 Mn1 115.8(5) . . ? C2 O14 Mo4 121.5(5) . . ? Mn1 O14 Mo4 101.5(2) . . ? C2 O14 Mo3 121.2(4) . . ? Mn1 O14 Mo3 100.8(3) . . ? Mo4 O14 Mo3 91.32(18) . . ? Mo5 O16 Mo4 122.4(3) . . ? C13 O17 Mn1 117.8(5) . . ? C13 O17 Mo4 119.0(4) . . ? Mn1 O17 Mo4 102.8(2) . . ? C13 O17 Mo5 120.8(5) . . ? Mn1 O17 Mo5 101.7(2) . . ? Mo4 O17 Mo5 89.93(19) . . ? C3 O18 Mn1 116.4(5) . . ? C3 O18 Mo5 121.1(5) . . ? Mn1 O18 Mo5 99.4(2) . . ? C3 O18 Mo6 126.4(5) . . ? Mn1 O18 Mo6 97.6(2) . . ? Mo5 O18 Mo6 89.65(17) . . ? Mo6 O19 Mo5 123.7(3) . . ? C5 N1 C1 128.7(7) . . ? C16 N2 C12 126.8(8) . . ? C23 N3 C31 109.5(7) . . ? C23 N3 C35 112.2(8) . . ? C31 N3 C35 113.1(8) . . ? C23 N3 C27 107.1(8) . . ? C31 N3 C27 110.3(7) . . ? C35 N3 C27 104.4(7) . . ? C43 N4 C47 111.1(7) . . ? C43 N4 C39 109.7(7) . . ? C47 N4 C39 112.5(7) . . ? C43 N4 C51 106.9(7) . . ? C47 N4 C51 109.5(7) . . ? C39 N4 C51 106.8(7) . . ? C59 N5 C55 110.0(9) . . ? C59 N5 C63 109.6(8) . . ? C55 N5 C63 106.3(7) . . ? C59 N5 C67 107.6(7) . . ? C55 N5 C67 110.0(9) . . ? C63 N5 C67 113.2(9) . . ? C72 N6 C71 116.9(17) . . ? C72 N6 C73 132(2) . . ? C71 N6 C73 102(2) . . ? C74 N7 C75 112.5(11) . . ? C74 N7 C76 122.0(11) . . ? C75 N7 C76 125.2(11) . . ? C77 N8 C78 117.9(13) . . ? C77 N8 C79 124.9(9) . . ? C78 N8 C79 117.1(12) . . ? N1 C1 C4 107.2(6) . . ? N1 C1 C2 102.0(7) . . ? C4 C1 C2 113.3(7) . . ? N1 C1 C3 109.0(7) . . ? C4 C1 C3 111.5(7) . . ? C2 C1 C3 113.2(7) . . ? O14 C2 C1 113.6(7) . . ? O18 C3 C1 114.3(7) . . ? O3 C4 C1 113.4(6) . . ? O25 C5 N1 121.0(9) . . ? O25 C5 C6 120.3(7) . . ? N1 C5 C6 118.6(7) . . ? C7 C6 C11 120.0 . . ? C7 C6 C5 123.1(4) . . ? C11 C6 C5 116.8(4) . . ? C8 C7 C6 120.0 . . ? C7 C8 C9 120.0 . . ? C8 C9 C10 120.0 . . ? C9 C10 C11 120.0 . . ? C10 C11 C6 120.0 . . ? N2 C12 C15 106.3(7) . . ? N2 C12 C14 109.0(7) . . ? C15 C12 C14 109.8(7) . . ? N2 C12 C13 108.9(7) . . ? C15 C12 C13 111.7(7) . . ? C14 C12 C13 111.0(7) . . ? O17 C13 C12 113.7(7) . . ? O10 C14 C12 112.0(7) . . ? O2 C15 C12 116.0(7) . . ? O26 C16 N2 125.6(10) . . ? O26 C16 C17 115.1(8) . . ? N2 C16 C17 119.3(9) . . ? C18 C17 C22 120.0 . . ? C18 C17 C16 117.6(5) . . ? C22 C17 C16 122.4(5) . . ? C17 C18 C19 120.0 . . ? C20 C19 C18 120.0 . . ? C21 C20 C19 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C17 120.0 . . ? N3 C23 C24 121.4(8) . . ? C25 C24 C23 111.0(8) . . ? C24 C25 C26 110.9(9) . . ? C28 C27 N3 113.4(8) . . ? C27 C28 C29 112.6(10) . . ? C30 C29 C28 115.1(12) . . ? C32 C31 N3 113.3(8) . . ? C31 C32 C33 108.9(9) . . ? C32 C33 C34 111.2(9) . . ? C36 C35 N3 117.3(9) . . ? C35 C36 C37 101.2(11) . . ? C38 C37 C36 105.8(13) . . ? C40 C39 N4 117.1(7) . . ? C41 C40 C39 110.2(9) . . ? C42 C41 C40 96.7(11) . . ? N4 C43 C44 118.2(8) . . ? C43 C44 C45 113.1(9) . . ? C46 C45 C44 112.7(12) . . ? C48 C47 N4 118.1(8) . . ? C47 C48 C49 111.5(9) . . ? C50 C49 C48 115.5(17) . . ? C52 C51 N4 115.8(8) . . ? C53 C52 C51 114.4(10) . . ? C54 C53 C52 124(2) . . ? C56 C55 N5 115.9(9) . . ? C55 C56 C57 111.2(9) . . ? C58 C57 C56 115.7(10) . . ? N5 C59 C60 113.3(9) . . ? C61 C60 C59 111.9(10) . . ? C62 C61 C60 121.0(15) . . ? N5 C63 C64 117.0(8) . . ? C65 C64 C63 111.5(10) . . ? C66 C65 C64 115.5(16) . . ? C68 C67 N5 110.7(9) . . ? C69 C68 C67 103.7(10) . . ? C68 C69 C70 109.9(11) . . ? O27 C71 N6 133.2(15) . . ? O28 C74 N7 114.8(12) . . ? O29 C77 N8 126.0(14) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.82 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.98 _refine_diff_density_min -1.02 _refine_diff_density_rms 0.15 data_mh192 _database_code_depnum_ccdc_archive 'CCDC 909165' #TrackingRef 'MnMo6-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H138 Mn Mo6 N7 O30' _chemical_formula_weight 2164.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 28.3641(5) _cell_length_b 23.7876(5) _cell_length_c 15.0216(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10135.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17042 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 25.6 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4448 _exptl_absorpt_coefficient_mu 0.908 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7917 _exptl_absorpt_correction_T_max 0.8610 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w & \p scans' _diffrn_detector_area_resol_mean 10.4383 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 78055 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.69 _reflns_number_total 9622 _reflns_number_gt 7561 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics diamond3 _computing_publication_material WinGX _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^ > 2\s(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^)+(0.0594P)^2^+20.8270P] 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 none _refine_ls_number_reflns 9622 _refine_ls_number_parameters 494 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1211 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.066 _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 0.085150(13) 0.939154(16) 0.12634(3) 0.02859(12) Uani 1 1 d . A 1 Mo2 Mo 0.009505(14) 0.860633(16) 0.00672(3) 0.03274(12) Uani 1 1 d . A 1 Mo3 Mo 0.076099(14) 1.079116(16) 0.11577(3) 0.03040(12) Uani 1 1 d . . 1 Mn1 Mn 0.0000 1.0000 0.0000 0.0238(2) Uani 1 2 d S . 1 O1 O -0.01741(11) 0.88100(13) -0.1057(2) 0.0344(8) Uani 1 1 d . . 1 O2 O -0.03153(12) 0.81526(14) 0.0465(2) 0.0450(9) Uani 1 1 d . A 1 O3 O 0.05478(12) 0.81986(14) -0.0304(2) 0.0451(9) Uani 1 1 d . A 1 O4 O 0.03319(11) 0.88821(12) 0.1183(2) 0.0317(7) Uani 1 1 d . A 1 O5 O 0.13041(11) 0.89819(14) 0.0890(3) 0.0427(9) Uani 1 1 d . A 1 O6 O 0.09164(11) 0.94137(14) 0.2387(2) 0.0401(8) Uani 1 1 d . A 1 O7 O 0.08461(11) 1.08614(14) 0.2273(2) 0.0404(8) Uani 1 1 d . B 1 O8 O 0.10858(10) 1.01070(12) 0.0873(2) 0.0300(7) Uani 1 1 d . A 1 O9 O 0.11418(12) 1.12519(14) 0.0665(2) 0.0432(9) Uani 1 1 d . C 1 O10 O -0.04082(10) 0.93858(12) 0.0287(2) 0.0280(7) Uani 1 1 d . . 1 O11 O 0.05018(10) 0.94475(12) -0.0202(2) 0.0292(7) Uani 1 1 d . A 1 O12 O 0.02393(10) 1.00519(12) 0.1303(2) 0.0280(7) Uani 1 1 d . A 1 O13 O -0.16302(13) 0.9720(2) 0.1766(3) 0.0606(11) Uani 1 1 d . D 1 O14 O -0.1469(7) 0.8990(8) 0.3630(12) 0.096(5) Uiso 0.35 1 d P D 1 O15 O -0.2246(5) 0.8751(5) 0.3723(8) 0.105(4) Uiso 0.50 1 d P D 1 O14' O -0.1280(4) 0.8733(4) 0.3280(7) 0.079(3) Uiso 0.50 1 d P E 2 O15' O -0.1984(3) 0.8338(4) 0.3261(6) 0.074(3) Uiso 0.50 1 d P E 2 N1 N -0.09276(14) 0.99782(18) 0.2377(3) 0.0422(10) Uani 1 1 d . D 1 H1 H -0.0790 1.0067 0.2883 0.051 Uiso 1 1 calc R D 1 N2 N 0.9812(3) 0.7500 0.7500 0.064(2) Uani 1 2 d S . 1 N3 N 0.2500 0.0000 0.0393(5) 0.067(2) Uani 1 2 d S . 1 N4 N 0.0877(2) 0.7500 0.2500 0.0483(16) Uani 1 2 d S . 1 N5 N 0.0547(2) 0.9864(3) 0.5674(4) 0.089(2) Uani 1 1 d . F 1 C1 C -0.01218(15) 1.0053(2) 0.1957(3) 0.0338(11) Uani 1 1 d . A 1 H1A H -0.0108 1.0412 0.2290 0.041 Uiso 1 1 calc R A 1 H1B H -0.0060 0.9745 0.2385 0.041 Uiso 1 1 calc R A 1 C2 C 0.07852(16) 0.9522(2) -0.0990(3) 0.0344(11) Uani 1 1 d . . 1 H2A H 0.0772 0.9173 -0.1349 0.041 Uiso 1 1 calc R . 1 H2B H 0.1117 0.9581 -0.0810 0.041 Uiso 1 1 calc R . 1 C3 C -0.06256(16) 0.9980(2) 0.1572(3) 0.0319(10) Uani 1 1 d . . 1 C4 C -0.06792(17) 0.9411(2) 0.1094(3) 0.0337(11) Uani 1 1 d . G 1 H4A H -0.0576 0.9107 0.1498 0.040 Uiso 1 1 calc R G 1 H4B H -0.1016 0.9349 0.0952 0.040 Uiso 1 1 calc R G 1 C5 C -0.1392(2) 0.9855(3) 0.2412(4) 0.0575(16) Uani 1 1 d D D 1 C6 C -0.1634(5) 1.0024(6) 0.3303(9) 0.047(4) Uani 0.50 1 d PD D 1 H6A H -0.1407 0.9988 0.3801 0.057 Uiso 1 1 calc R D 1 H6B H -0.1740 1.0420 0.3273 0.057 Uiso 1 1 calc R D 1 C7 C -0.2046(5) 0.9647(7) 0.3454(10) 0.082(5) Uani 0.50 1 d PD D 1 H7A H -0.2213 0.9759 0.4004 0.099 Uiso 1 1 calc R D 1 H7B H -0.2268 0.9676 0.2949 0.099 Uiso 1 1 calc R D 1 C8 C -0.1874(7) 0.9070(8) 0.3535(12) 0.047(5) Uiso 0.35 1 d PD D 1 C6' C -0.1588(6) 0.9747(6) 0.3338(10) 0.050(4) Uani 0.50 1 d PD E 2 C7' C -0.1950(5) 0.9299(6) 0.3471(9) 0.044(3) Uiso 0.50 1 d PD E 2 C8' C -0.1667(5) 0.8795(5) 0.3308(8) 0.049(3) Uiso 0.50 1 d PD E 2 C9 C 0.9501(3) 0.7566(3) 0.8328(5) 0.0709(19) Uani 1 1 d . . 1 H9A H 0.9708 0.7623 0.8851 0.085 Uiso 1 1 calc R . 1 H9B H 0.9307 0.7908 0.8258 0.085 Uiso 1 1 calc R . 1 C10 C 0.9177(3) 0.7072(3) 0.8516(6) 0.091(3) Uani 1 1 d . . 1 H10A H 0.9010 0.6966 0.7962 0.110 Uiso 1 1 calc R . 1 H10B H 0.9367 0.6746 0.8711 0.110 Uiso 1 1 calc R . 1 C11 C 0.8824(3) 0.7213(3) 0.9218(6) 0.094(3) Uani 1 1 d . . 1 H11A H 0.8618 0.7519 0.9001 0.112 Uiso 1 1 calc R . 1 H11B H 0.8991 0.7351 0.9754 0.112 Uiso 1 1 calc R . 1 C12 C 0.8526(3) 0.6717(4) 0.9466(6) 0.104(3) Uiso 1 1 d . . 1 H12A H 0.8369 0.6570 0.8933 0.156 Uiso 1 1 calc R . 1 H12B H 0.8289 0.6832 0.9903 0.156 Uiso 1 1 calc R . 1 H12C H 0.8727 0.6423 0.9724 0.156 Uiso 1 1 calc R . 1 C13 C 1.0110(2) 0.8028(3) 0.7435(4) 0.0649(18) Uani 1 1 d . . 1 H13A H 0.9899 0.8356 0.7359 0.078 Uiso 1 1 calc R . 1 H13B H 1.0284 0.8079 0.8001 0.078 Uiso 1 1 calc R . 1 C14 C 1.0459(3) 0.8017(3) 0.6675(5) 0.083(2) Uani 1 1 d . . 1 H14A H 1.0649 0.7667 0.6705 0.100 Uiso 1 1 calc R . 1 H14B H 1.0288 0.8019 0.6101 0.100 Uiso 1 1 calc R . 1 C15 C 1.0781(3) 0.8520(4) 0.6726(7) 0.102(3) Uiso 1 1 d . . 1 H15A H 1.0589 0.8863 0.6645 0.123 Uiso 1 1 calc R . 1 H15B H 1.0920 0.8535 0.7330 0.123 Uiso 1 1 calc R . 1 C16 C 1.1175(4) 0.8527(5) 0.6057(8) 0.154(5) Uiso 1 1 d . . 1 H16A H 1.1341 0.8166 0.6070 0.231 Uiso 1 1 calc R . 1 H16B H 1.1395 0.8830 0.6203 0.231 Uiso 1 1 calc R . 1 H16C H 1.1045 0.8590 0.5461 0.231 Uiso 1 1 calc R . 1 C17 C 0.21534(19) -0.0329(3) -0.0183(4) 0.0615(17) Uani 1 1 d . H 1 H17A H 0.1903 -0.0482 0.0206 0.074 Uiso 1 1 calc R H 1 H17B H 0.2002 -0.0065 -0.0605 0.074 Uiso 1 1 calc R H 1 C18 C 0.2364(2) -0.0807(3) -0.0708(6) 0.075(2) Uani 1 1 d . H 1 H18A H 0.2598 -0.0658 -0.1137 0.090 Uiso 1 1 calc R H 1 H18B H 0.2529 -0.1068 -0.0300 0.090 Uiso 1 1 calc R H 1 C19 C 0.1982(2) -0.1116(3) -0.1200(5) 0.079(2) Uani 1 1 d . H 1 H19A H 0.1827 -0.0851 -0.1615 0.095 Uiso 1 1 calc R H 1 H19B H 0.1742 -0.1242 -0.0765 0.095 Uiso 1 1 calc R H 1 C20 C 0.2149(3) -0.1619(4) -0.1719(6) 0.103(3) Uiso 1 1 d . H 1 H20A H 0.2327 -0.1492 -0.2241 0.155 Uiso 1 1 calc R H 1 H20B H 0.1877 -0.1840 -0.1913 0.155 Uiso 1 1 calc R H 1 H20C H 0.2353 -0.1851 -0.1341 0.155 Uiso 1 1 calc R H 1 C21 C 0.2194(3) 0.0469(4) 0.0904(7) 0.048(3) Uiso 0.60 1 d P I 1 H21A H 0.2011 0.0679 0.0452 0.058 Uiso 1 1 calc R I 1 H21B H 0.1964 0.0271 0.1288 0.058 Uiso 1 1 calc R I 1 C22 C 0.2447(4) 0.0889(5) 0.1470(8) 0.062(3) Uiso 0.60 1 d P I 1 H22A H 0.2623 0.0689 0.1942 0.074 Uiso 1 1 calc R I 1 H22B H 0.2679 0.1093 0.1098 0.074 Uiso 1 1 calc R I 1 C23 C 0.2135(5) 0.1288(7) 0.1874(10) 0.071(4) Uiso 0.60 1 d P I 1 H23A H 0.1903 0.1080 0.2242 0.085 Uiso 1 1 calc R I 1 H23B H 0.1957 0.1482 0.1397 0.085 Uiso 1 1 calc R I 1 C24 C 0.2366(5) 0.1720(6) 0.2441(10) 0.097(4) Uiso 0.60 1 d P I 1 H24A H 0.2494 0.1541 0.2977 0.145 Uiso 1 1 calc R I 1 H24B H 0.2133 0.2005 0.2614 0.145 Uiso 1 1 calc R I 1 H24C H 0.2622 0.1899 0.2108 0.145 Uiso 1 1 calc R I 1 C21' C 0.2222(5) 0.0228(7) 0.1051(10) 0.043(3) Uiso 0.40 1 d P . 2 C22' C 0.2506(5) 0.0566(7) 0.1719(11) 0.055(4) Uiso 0.40 1 d P J 2 C23' C 0.2184(8) 0.0979(10) 0.2258(17) 0.097(7) Uiso 0.40 1 d P J 2 C24' C 0.2110(11) 0.1559(13) 0.182(2) 0.117(10) Uiso 0.40 1 d P J 2 C25 C 0.1174(2) 0.7710(2) 0.1735(4) 0.0509(14) Uani 1 1 d . . 1 H25A H 0.0960 0.7832 0.1251 0.061 Uiso 1 1 calc R . 1 H25B H 0.1350 0.8045 0.1938 0.061 Uiso 1 1 calc R . 1 C26 C 0.1521(2) 0.7296(3) 0.1355(4) 0.0642(17) Uani 1 1 d . . 1 H26A H 0.1354 0.6950 0.1170 0.077 Uiso 1 1 calc R . 1 H26B H 0.1756 0.7194 0.1813 0.077 Uiso 1 1 calc R . 1 C27 C 0.1766(3) 0.7557(3) 0.0559(5) 0.084(2) Uiso 1 1 d . . 1 H27A H 0.1891 0.7931 0.0730 0.101 Uiso 1 1 calc R . 1 H27B H 0.1533 0.7615 0.0077 0.101 Uiso 1 1 calc R . 1 C28 C 0.2169(4) 0.7198(4) 0.0207(7) 0.131(4) Uiso 1 1 d . . 1 H28A H 0.2401 0.7139 0.0681 0.196 Uiso 1 1 calc R . 1 H28B H 0.2320 0.7391 -0.0294 0.196 Uiso 1 1 calc R . 1 H28C H 0.2045 0.6835 0.0008 0.196 Uiso 1 1 calc R . 1 C29 C 0.0580(2) 0.8006(3) 0.2787(4) 0.0637(18) Uani 1 1 d D . 1 H29A H 0.0349 0.8079 0.2307 0.076 Uiso 1 1 calc R . 1 H29B H 0.0793 0.8335 0.2811 0.076 Uiso 1 1 calc R . 1 C30 C 0.0306(4) 0.7988(4) 0.3669(7) 0.039(3) Uiso 0.50 1 d PD . 1 H30A H 0.0525 0.7996 0.4183 0.047 Uiso 1 1 calc R . 1 H30B H 0.0111 0.7644 0.3707 0.047 Uiso 1 1 calc R . 1 C31 C -0.0014(10) 0.8527(11) 0.3660(18) 0.122(12) Uiso 0.50 1 d PD . 1 H31A H 0.0183 0.8870 0.3611 0.146 Uiso 1 1 calc R . 1 H31B H -0.0232 0.8516 0.3146 0.146 Uiso 1 1 calc R . 1 C32 C -0.0279(7) 0.8533(9) 0.4494(13) 0.097(6) Uiso 0.40 1 d PD . 1 H32A H -0.0433 0.8168 0.4580 0.145 Uiso 1 1 calc R . 1 H32B H -0.0519 0.8829 0.4471 0.145 Uiso 1 1 calc R . 1 H32C H -0.0064 0.8606 0.4991 0.145 Uiso 1 1 calc R . 1 C30' C 0.0211(5) 0.7805(7) 0.3411(11) 0.078(5) Uiso 0.50 1 d PD K 2 C31' C -0.0130(9) 0.8274(10) 0.359(2) 0.062(7) Uiso 0.25 1 d PD K 2 C32' C 0.0144(12) 0.8739(14) 0.406(2) 0.103(12) Uiso 0.30 1 d PD K 2 C33 C 0.0586(3) 1.0039(3) 0.4973(5) 0.0665(18) Uiso 1 1 d . F 1 C34 C 0.0622(3) 1.0277(3) 0.4071(5) 0.080(2) Uiso 1 1 d . F 1 H34A H 0.0676 0.9973 0.3642 0.121 Uiso 1 1 calc R F 1 H34B H 0.0886 1.0542 0.4048 0.121 Uiso 1 1 calc R F 1 H34C H 0.0329 1.0473 0.3923 0.121 Uiso 1 1 calc R F 1 C8" C -0.2214(11) 0.9315(13) 0.421(2) 0.037(7) Uiso 0.15 1 d P L 3 O14" O -0.2602(13) 0.9065(15) 0.410(3) 0.089(10) Uiso 0.15 1 d P L 3 C31" C 0.0019(13) 0.850(2) 0.392(3) 0.074(12) Uiso 0.25 1 d PD M 3 C32" C -0.0394(12) 0.8486(15) 0.330(2) 0.113(11) Uiso 0.30 1 d PD M 3 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 0.0257(2) 0.0298(2) 0.0302(2) 0.00223(16) -0.00502(16) -0.00144(15) Mo2 0.0355(2) 0.0261(2) 0.0367(3) -0.00036(17) -0.00978(18) -0.00160(16) Mo3 0.0293(2) 0.0284(2) 0.0335(2) -0.00063(16) -0.00726(17) -0.00480(15) Mn1 0.0234(5) 0.0251(5) 0.0228(5) 0.0003(4) -0.0014(4) -0.0027(4) O1 0.0425(19) 0.0273(17) 0.0333(19) -0.0041(14) -0.0090(15) 0.0009(14) O2 0.049(2) 0.0326(19) 0.053(2) 0.0081(16) -0.0130(18) -0.0107(16) O3 0.046(2) 0.0392(19) 0.050(2) -0.0075(16) -0.0134(18) 0.0069(16) O4 0.0346(17) 0.0275(17) 0.0331(18) 0.0041(13) -0.0053(14) -0.0017(13) O5 0.0313(18) 0.0378(19) 0.059(2) 0.0001(17) -0.0034(17) 0.0035(15) O6 0.0388(19) 0.046(2) 0.035(2) 0.0040(16) -0.0069(15) -0.0075(15) O7 0.0410(19) 0.042(2) 0.039(2) -0.0059(16) -0.0078(16) -0.0016(15) O8 0.0255(16) 0.0303(17) 0.0343(18) 0.0009(13) -0.0040(14) -0.0036(12) O9 0.041(2) 0.0381(19) 0.050(2) 0.0050(16) -0.0098(17) -0.0106(15) O10 0.0259(15) 0.0302(16) 0.0279(17) 0.0008(13) -0.0022(13) -0.0045(12) O11 0.0276(16) 0.0330(17) 0.0268(17) -0.0003(13) 0.0018(13) -0.0026(13) O12 0.0254(16) 0.0307(16) 0.0278(18) -0.0009(13) 0.0028(13) -0.0030(12) O13 0.034(2) 0.111(4) 0.036(2) 0.002(2) 0.0003(18) -0.015(2) N1 0.031(2) 0.071(3) 0.025(2) 0.002(2) 0.0035(18) -0.004(2) N2 0.098(6) 0.033(4) 0.060(5) -0.013(3) 0.000 0.000 N3 0.025(3) 0.118(7) 0.058(5) 0.000 0.000 -0.016(4) N4 0.049(4) 0.041(4) 0.055(4) 0.018(3) 0.000 0.000 N5 0.090(5) 0.128(6) 0.049(4) 0.014(4) -0.011(3) 0.006(4) C1 0.026(2) 0.050(3) 0.026(3) -0.002(2) 0.003(2) -0.004(2) C2 0.028(2) 0.048(3) 0.028(3) 0.000(2) 0.003(2) 0.002(2) C3 0.027(2) 0.045(3) 0.023(2) 0.000(2) 0.0057(19) -0.004(2) C4 0.032(2) 0.042(3) 0.028(3) 0.005(2) 0.002(2) -0.004(2) C5 0.038(3) 0.095(5) 0.040(4) 0.002(3) 0.009(3) -0.007(3) C6 0.037(7) 0.075(12) 0.029(7) -0.011(8) 0.014(5) 0.002(8) C7 0.054(9) 0.144(16) 0.049(9) 0.021(10) 0.034(7) 0.007(10) C6' 0.044(8) 0.054(10) 0.052(8) 0.000(8) 0.007(6) -0.004(8) C9 0.104(5) 0.045(4) 0.063(5) -0.020(3) 0.012(4) -0.013(4) C10 0.119(7) 0.056(4) 0.099(6) -0.030(4) 0.015(5) -0.026(4) C11 0.113(6) 0.062(5) 0.106(7) -0.016(4) 0.024(5) -0.030(4) C13 0.094(5) 0.045(3) 0.056(4) -0.017(3) 0.011(4) -0.008(3) C14 0.121(7) 0.053(4) 0.074(5) -0.018(4) 0.033(5) 0.001(4) C17 0.027(3) 0.099(5) 0.058(4) 0.003(4) 0.002(3) -0.008(3) C18 0.037(3) 0.099(5) 0.089(6) 0.010(4) 0.002(4) 0.001(3) C19 0.053(4) 0.098(6) 0.087(6) -0.017(4) 0.002(4) 0.011(4) C25 0.052(3) 0.046(3) 0.055(4) 0.015(3) 0.001(3) 0.000(3) C26 0.068(4) 0.069(4) 0.055(4) 0.013(3) 0.008(3) 0.012(3) C29 0.054(4) 0.058(4) 0.079(5) 0.029(3) 0.018(3) 0.011(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O6 1.699(3) . ? Mo1 O5 1.706(3) . ? Mo1 O4 1.912(3) . ? Mo1 O8 1.919(3) . ? Mo1 O12 2.342(3) . ? Mo1 O11 2.418(3) . ? Mo2 O2 1.696(3) . ? Mo2 O3 1.703(3) . ? Mo2 O1 1.916(3) . ? Mo2 O4 1.921(3) . ? Mo2 O11 2.345(3) . ? Mo2 O10 2.363(3) . ? Mo3 O7 1.701(3) . ? Mo3 O9 1.707(3) . ? Mo3 O8 1.918(3) . ? Mo3 O1 1.922(3) 5_575 ? Mo3 O12 2.309(3) . ? Mo3 O10 2.426(3) 5_575 ? Mn1 O10 1.913(3) 5_575 ? Mn1 O10 1.913(3) . ? Mn1 O11 1.961(3) 5_575 ? Mn1 O11 1.961(3) . ? Mn1 O12 2.075(3) 5_575 ? Mn1 O12 2.075(3) . ? O1 Mo3 1.922(3) 5_575 ? O10 C4 1.437(5) . ? O10 Mo3 2.426(3) 5_575 ? O11 C2 1.441(5) . ? O12 C1 1.419(5) . ? O13 C5 1.226(7) . ? O14 C8 1.17(2) . ? O15 C8 1.33(2) . ? O14' C8' 1.110(15) . ? O15' C8' 1.412(15) . ? N1 C5 1.350(7) . ? N1 C3 1.482(6) . ? N2 C13 1.518(7) . ? N2 C13 1.518(7) 4_566 ? N2 C9 1.532(8) 4_566 ? N2 C9 1.532(8) . ? N3 C17 1.526(7) 2 ? N3 C17 1.526(7) . ? N3 C21 1.608(10) . ? N3 C21 1.608(10) 2 ? N4 C25 1.509(6) . ? N4 C25 1.509(6) 4_565 ? N4 C29 1.530(7) 4_565 ? N4 C29 1.530(7) . ? N5 C33 1.138(9) . ? C1 C3 1.551(6) . ? C2 C3 1.541(7) 5_575 ? C3 C4 1.539(7) . ? C3 C2 1.541(7) 5_575 ? C5 C6 1.557(12) . ? C6 C7 1.491(15) . ? C7 C8 1.460(16) . ? C6' C7' 1.492(15) . ? C7' C8' 1.465(14) . ? C9 C10 1.517(9) . ? C10 C11 1.491(11) . ? C11 C12 1.499(10) . ? C13 C14 1.513(9) . ? C14 C15 1.506(11) . ? C15 C16 1.502(13) . ? C17 C18 1.507(9) . ? C18 C19 1.503(10) . ? C19 C20 1.504(10) . ? C21 C22 1.496(14) . ? C22 C23 1.434(16) . ? C23 C24 1.487(19) . ? C21' C22' 1.52(2) . ? C21' C21' 1.91(3) 2 ? C22' C23' 1.57(3) . ? C23' C24' 1.54(4) . ? C25 C26 1.504(8) . ? C26 C27 1.517(9) . ? C27 C28 1.520(12) . ? C29 C30 1.538(10) . ? C30 C31 1.571(17) . ? C31 C32 1.462(17) . ? C30' C31' 1.502(17) . ? C31' C32' 1.522(19) . ? C33 C34 1.471(10) . ? C8" O14" 1.26(5) . ? C31" C32" 1.50(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Mo1 O5 105.24(17) . . ? O6 Mo1 O4 99.57(14) . . ? O5 Mo1 O4 101.37(15) . . ? O6 Mo1 O8 103.80(15) . . ? O5 Mo1 O8 98.37(15) . . ? O4 Mo1 O8 144.08(13) . . ? O6 Mo1 O12 91.97(14) . . ? O5 Mo1 O12 161.61(15) . . ? O4 Mo1 O12 81.68(12) . . ? O8 Mo1 O12 70.71(11) . . ? O6 Mo1 O11 161.31(13) . . ? O5 Mo1 O11 92.33(14) . . ? O4 Mo1 O11 70.17(12) . . ? O8 Mo1 O11 79.36(12) . . ? O12 Mo1 O11 71.46(10) . . ? O2 Mo2 O3 105.68(17) . . ? O2 Mo2 O1 101.41(15) . . ? O3 Mo2 O1 98.97(16) . . ? O2 Mo2 O4 98.64(16) . . ? O3 Mo2 O4 102.50(15) . . ? O1 Mo2 O4 145.30(13) . . ? O2 Mo2 O11 160.30(15) . . ? O3 Mo2 O11 93.36(14) . . ? O1 Mo2 O11 80.11(12) . . ? O4 Mo2 O11 71.75(11) . . ? O2 Mo2 O10 92.04(14) . . ? O3 Mo2 O10 161.45(14) . . ? O1 Mo2 O10 71.58(12) . . ? O4 Mo2 O10 79.71(12) . . ? O11 Mo2 O10 69.62(10) . . ? O7 Mo3 O9 105.88(17) . . ? O7 Mo3 O8 103.56(15) . . ? O9 Mo3 O8 98.31(15) . . ? O7 Mo3 O1 98.74(15) . 5_575 ? O9 Mo3 O1 101.36(15) . 5_575 ? O8 Mo3 O1 144.81(13) . 5_575 ? O7 Mo3 O12 94.17(14) . . ? O9 Mo3 O12 159.31(14) . . ? O8 Mo3 O12 71.49(11) . . ? O1 Mo3 O12 80.11(12) 5_575 . ? O7 Mo3 O10 163.04(13) . 5_575 ? O9 Mo3 O10 89.14(14) . 5_575 ? O8 Mo3 O10 81.48(12) . 5_575 ? O1 Mo3 O10 70.01(12) 5_575 5_575 ? O12 Mo3 O10 71.83(10) . 5_575 ? O10 Mn1 O10 180.000(1) 5_575 . ? O10 Mn1 O11 87.83(12) 5_575 5_575 ? O10 Mn1 O11 92.17(12) . 5_575 ? O10 Mn1 O11 92.17(12) 5_575 . ? O10 Mn1 O11 87.83(12) . . ? O11 Mn1 O11 180.0 5_575 . ? O10 Mn1 O12 91.77(12) 5_575 5_575 ? O10 Mn1 O12 88.23(12) . 5_575 ? O11 Mn1 O12 87.04(12) 5_575 5_575 ? O11 Mn1 O12 92.96(12) . 5_575 ? O10 Mn1 O12 88.23(12) 5_575 . ? O10 Mn1 O12 91.77(12) . . ? O11 Mn1 O12 92.96(12) 5_575 . ? O11 Mn1 O12 87.04(12) . . ? O12 Mn1 O12 180.000(1) 5_575 . ? Mo2 O1 Mo3 122.64(17) . 5_575 ? Mo1 O4 Mo2 122.78(16) . . ? Mo3 O8 Mo1 121.22(16) . . ? C4 O10 Mn1 118.8(3) . . ? C4 O10 Mo2 118.3(3) . . ? Mn1 O10 Mo2 101.66(12) . . ? C4 O10 Mo3 122.8(2) . 5_575 ? Mn1 O10 Mo3 100.40(12) . 5_575 ? Mo2 O10 Mo3 89.32(10) . 5_575 ? C2 O11 Mn1 116.7(3) . . ? C2 O11 Mo2 121.4(3) . . ? Mn1 O11 Mo2 100.85(12) . . ? C2 O11 Mo1 121.7(2) . . ? Mn1 O11 Mo1 101.18(12) . . ? Mo2 O11 Mo1 89.88(10) . . ? C1 O12 Mn1 114.6(3) . . ? C1 O12 Mo3 121.8(3) . . ? Mn1 O12 Mo3 99.55(12) . . ? C1 O12 Mo1 123.6(3) . . ? Mn1 O12 Mo1 100.29(12) . . ? Mo3 O12 Mo1 91.91(10) . . ? C5 N1 C3 126.6(4) . . ? C13 N2 C13 112.2(7) . 4_566 ? C13 N2 C9 110.7(4) . 4_566 ? C13 N2 C9 106.7(3) 4_566 4_566 ? C13 N2 C9 106.7(3) . . ? C13 N2 C9 110.7(4) 4_566 . ? C9 N2 C9 109.9(8) 4_566 . ? C17 N3 C17 110.9(7) 2 . ? C17 N3 C21 105.2(5) 2 . ? C17 N3 C21 106.2(4) . . ? C17 N3 C21 106.2(4) 2 2 ? C17 N3 C21 105.2(5) . 2 ? C21 N3 C21 122.9(10) . 2 ? C25 N4 C25 112.2(6) . 4_565 ? C25 N4 C29 110.6(4) . 4_565 ? C25 N4 C29 105.1(3) 4_565 4_565 ? C25 N4 C29 105.1(3) . . ? C25 N4 C29 110.6(4) 4_565 . ? C29 N4 C29 113.3(6) 4_565 . ? O12 C1 C3 114.0(4) . . ? O11 C2 C3 113.3(4) . 5_575 ? N1 C3 C4 108.7(4) . . ? N1 C3 C2 107.2(4) . 5_575 ? C4 C3 C2 112.5(4) . 5_575 ? N1 C3 C1 103.2(4) . . ? C4 C3 C1 111.3(4) . . ? C2 C3 C1 113.3(4) 5_575 . ? O10 C4 C3 112.2(4) . . ? O13 C5 N1 124.3(5) . . ? O13 C5 C6 120.3(7) . . ? N1 C5 C6 114.0(7) . . ? C7 C6 C5 108.7(10) . . ? C8 C7 C6 108.5(12) . . ? O14 C8 O15 131.2(19) . . ? O14 C8 C7 119.2(17) . . ? O15 C8 C7 106.9(15) . . ? C8' C7' C6' 100.6(10) . . ? O14' C8' O15' 121.7(12) . . ? O14' C8' C7' 131.2(13) . . ? O15' C8' C7' 106.9(10) . . ? C10 C9 N2 114.8(5) . . ? C11 C10 C9 111.4(6) . . ? C10 C11 C12 112.2(7) . . ? C14 C13 N2 113.5(5) . . ? C15 C14 C13 110.1(6) . . ? C16 C15 C14 115.1(8) . . ? C18 C17 N3 115.3(4) . . ? C19 C18 C17 109.9(5) . . ? C18 C19 C20 114.6(6) . . ? C22 C21 N3 118.4(8) . . ? C23 C22 C21 112.7(10) . . ? C22 C23 C24 115.3(11) . . ? C22' C21' C21' 82.0(10) . 2 ? C21' C22' C23' 111.3(14) . . ? C24' C23' C22' 115(2) . . ? C26 C25 N4 116.0(4) . . ? C25 C26 C27 109.4(5) . . ? C26 C27 C28 112.9(7) . . ? N4 C29 C30 120.0(5) . . ? C29 C30 C31 105.2(10) . . ? C32 C31 C30 107.3(16) . . ? C30' C31' C32' 107(2) . . ? N5 C33 C34 178.0(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.69 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.78 _refine_diff_density_min -0.52 _refine_diff_density_rms 0.10 data_mh222-twin5 _database_code_depnum_ccdc_archive 'CCDC 909166' #TrackingRef 'MnMo6-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H151 Mn Mo6 N10 O30' _chemical_formula_weight 2315.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 14.9246(8) _cell_length_b 17.3492(10) _cell_length_c 20.5931(11) _cell_angle_alpha 77.925(4) _cell_angle_beta 78.223(3) _cell_angle_gamma 74.076(3) _cell_volume 4952.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3298 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 22.9 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2388 _exptl_absorpt_coefficient_mu 0.935 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8881 _exptl_absorpt_correction_T_max 0.9547 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Oxford Gemini Ultra A CCD' _diffrn_measurement_method '\w & \p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 18771 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1263 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 26.00 _reflns_number_total 18773 _reflns_number_gt 12634 _reflns_threshold_expression >2\s(I) _computing_data_collection Apex2 _computing_cell_refinement Apex2 _computing_data_reduction Apex2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics diamond3 _computing_publication_material WinGX _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^ > 2\s(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^)+(0.0000P)^2^+82.4077P] 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 none _refine_ls_number_reflns 18773 _refine_ls_number_parameters 808 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1347 _refine_ls_R_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.1891 _refine_ls_wR_factor_gt 0.1661 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.005 _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 0.56211(8) 0.55250(7) 0.63047(6) 0.0177(3) Uani 1 1 d . . . Mo2 Mo 0.49589(9) 0.37912(7) 0.64928(6) 0.0171(3) Uani 1 1 d . . . Mo3 Mo 0.57047(9) 0.67207(7) 0.47887(6) 0.0194(3) Uani 1 1 d . . . Mo4 Mo 0.83851(8) 0.00061(7) 1.13779(6) 0.0177(3) Uani 1 1 d . . . Mo5 Mo 0.98035(9) 0.16322(7) 0.87835(6) 0.0188(3) Uani 1 1 d . . . Mo6 Mo 0.81641(8) 0.16436(7) 1.01505(6) 0.0186(3) Uani 1 1 d . . . Mn1 Mn 0.5000 0.5000 0.5000 0.0094(6) Uani 1 2 d S . . Mn2 Mn 1.0000 0.0000 1.0000 0.0119(6) Uani 1 2 d S . . O1 O 0.6799(7) 0.6826(7) 0.4832(5) 0.033(3) Uani 1 1 d . . . O2 O 0.4006(7) 0.3653(6) 0.6060(5) 0.023(2) Uani 1 1 d . . . O3 O 0.6717(7) 0.5638(5) 0.6363(5) 0.025(2) Uani 1 1 d . . . O4 O 0.5043(7) 0.7658(5) 0.4595(5) 0.027(2) Uani 1 1 d . . . O5 O 0.5155(6) 0.6495(5) 0.5719(5) 0.021(2) Uani 1 1 d . . . O6 O 0.6099(7) 0.5330(6) 0.5153(5) 0.022(2) Uani 1 1 d . . . O7 O 0.5909(6) 0.4371(5) 0.6429(4) 0.015(2) Uani 1 1 d . . . O8 O 0.4948(7) 0.5742(6) 0.7046(5) 0.027(2) Uani 1 1 d . . . O9 O 0.4437(6) 0.5116(5) 0.5985(4) 0.018(2) Uani 1 1 d . . . O10 O 0.4340(7) 0.3923(6) 0.7263(5) 0.028(2) Uani 1 1 d . . . O11 O 0.8115(7) 0.2618(6) 1.0194(5) 0.031(3) Uani 1 1 d . . . O12 O 0.5650(7) 0.2833(6) 0.6614(5) 0.029(2) Uani 1 1 d . . . O13 O 0.5513(6) 0.3878(5) 0.5314(4) 0.015(2) Uani 1 1 d . . . O14 O 0.7024(6) 0.1618(6) 1.0178(5) 0.025(2) Uani 1 1 d . . . O15 O 0.8390(6) 0.1113(5) 1.1042(4) 0.017(2) Uani 1 1 d . . . O16 O 0.8543(6) 0.1604(6) 0.9206(5) 0.026(2) Uani 1 1 d . . . O17 O 0.9848(6) 0.2616(6) 0.8784(5) 0.026(2) Uani 1 1 d . . . O18 O 0.9675(7) 0.1598(7) 0.7982(5) 0.034(3) Uani 1 1 d . . . O19 O 0.9630(9) 0.0601(8) 0.4330(7) 0.063(4) Uani 1 1 d . . . O20 O 0.7226(7) 0.0040(6) 1.1466(5) 0.028(2) Uani 1 1 d . . . O21 O 0.8563(7) -0.0052(6) 1.2172(5) 0.031(3) Uani 1 1 d . . . O22 O 0.8621(6) 0.0177(5) 1.0204(4) 0.0104(19) Uani 1 1 d . . . O23 O 0.8880(6) -0.1090(5) 1.1241(4) 0.017(2) Uani 1 1 d . . . O24 O 1.0003(6) -0.0168(6) 1.0951(4) 0.017(2) Uani 1 1 d . . . O25 O 0.9797(6) 0.1264(5) 0.9923(4) 0.018(2) Uani 1 1 d . . . O26 O 0.9431(8) -0.1820(8) 0.8349(7) 0.052(4) Uani 1 1 d . . . O27 O 0.8183(9) -0.3343(7) 0.6892(6) 0.055(3) Uiso 1 1 d . . . O28 O 0.6778(8) -0.3548(7) 0.7324(5) 0.043(3) Uiso 1 1 d . . . H28 H 0.6923 -0.3845 0.7026 0.065 Uiso 1 1 calc R . . O29 O 0.7744(7) 0.2636(6) 0.4041(5) 0.032(3) Uani 1 1 d . . . O30 O 1.0966(10) 0.0498(8) 0.4720(7) 0.069(4) Uiso 1 1 d . . . H30 H 1.0779 0.0139 0.5018 0.104 Uiso 1 1 calc R . . N1 N 0.8311(8) -0.1091(7) 0.9077(6) 0.026(3) Uani 1 1 d . . . H1 H 0.7703 -0.0974 0.9233 0.031 Uiso 1 1 calc R . . N2 N 0.7948(8) 0.3716(7) 0.4389(6) 0.023(3) Uani 1 1 d . . . H2 H 0.8379 0.3948 0.4439 0.027 Uiso 1 1 calc R . . N3 N 0.6307(9) 0.1915(8) 0.2842(6) 0.037(3) Uani 1 1 d . . . N4 N 0.7580(9) 0.7426(8) 0.2511(7) 0.033(3) Uani 1 1 d . . . N5 N 0.7036(16) 0.3776(14) 0.8205(10) 0.014(5) Uiso 0.50 1 d PD A 1 N5' N 0.670(2) 0.3614(16) 0.8308(12) 0.029(6) Uiso 0.50 1 d PD B 2 N6 N 0.0419(11) 0.5497(10) 0.5534(8) 0.057(4) Uiso 1 1 d . . . N7 N 0.6149(11) 0.9294(10) 0.9468(8) 0.057(4) Uiso 1 1 d . . . N8 N 0.8619(19) 0.1567(16) 0.5703(13) 0.123(9) Uiso 1 1 d . . . N9 N 0.8011(18) -0.0059(16) 0.7243(13) 0.114(8) Uiso 1 1 d . . . N10 N 1.0926(17) 0.4204(15) 0.9281(12) 0.112(8) Uiso 1 1 d . . . C1 C 0.8222(9) -0.0260(8) 0.9872(7) 0.020(3) Uiso 1 1 d . . . H1A H 0.7728 0.0132 0.9634 0.024 Uiso 1 1 calc R . . H1B H 0.7910 -0.0634 1.0217 0.024 Uiso 1 1 calc R . . C2 C 1.0393(9) 0.1485(7) 1.0260(6) 0.014(3) Uiso 1 1 d . . . H2A H 0.9998 0.1824 1.0594 0.016 Uiso 1 1 calc R . . H2B H 1.0770 0.1822 0.9930 0.016 Uiso 1 1 calc R . . C3 C 0.9459(9) -0.0243(8) 0.8786(6) 0.016(3) Uiso 1 1 d . . . H3A H 0.9890 -0.0605 0.8482 0.019 Uiso 1 1 calc R . . H3B H 0.9003 0.0163 0.8523 0.019 Uiso 1 1 calc R . . C4 C 0.8917(9) -0.0751(8) 0.9369(7) 0.019(3) Uiso 1 1 d . . . C5 C 0.8607(11) -0.1569(10) 0.8588(8) 0.033(4) Uani 1 1 d . . . C6 C 0.7821(11) -0.1801(12) 0.8385(10) 0.050(5) Uani 1 1 d . . . H6A H 0.7401 -0.1301 0.8180 0.060 Uiso 1 1 calc R . . H6B H 0.7446 -0.2034 0.8796 0.060 Uiso 1 1 calc R . . C7 C 0.8116(9) -0.2405(9) 0.7896(7) 0.025(3) Uani 1 1 d . . . H7A H 0.8601 -0.2880 0.8065 0.029 Uiso 1 1 calc R . . H7B H 0.8395 -0.2146 0.7454 0.029 Uiso 1 1 calc R . . C8 C 0.7265(11) -0.2687(11) 0.7813(9) 0.044(4) Uani 1 1 d . . . H8A H 0.7018 -0.2977 0.8251 0.052 Uiso 1 1 calc R . . H8B H 0.6762 -0.2204 0.7684 0.052 Uiso 1 1 calc R . . C9 C 0.7479(10) -0.3219(11) 0.7312(8) 0.039(4) Uani 1 1 d . . . C10 C 0.7009(9) 0.4862(8) 0.4896(7) 0.017(3) Uiso 1 1 d . . . H10A H 0.7383 0.4645 0.5268 0.020 Uiso 1 1 calc R . . H10B H 0.7341 0.5227 0.4557 0.020 Uiso 1 1 calc R . . C11 C 0.6512(10) 0.3526(8) 0.5069(7) 0.021(3) Uani 1 1 d . . . H11A H 0.6556 0.3056 0.4851 0.026 Uiso 1 1 calc R . . H11B H 0.6860 0.3325 0.5456 0.026 Uiso 1 1 calc R . . C12 C 0.3447(9) 0.5566(9) 0.6091(7) 0.028(4) Uani 1 1 d . . . H12A H 0.3397 0.6041 0.6303 0.034 Uiso 1 1 calc R . . H12B H 0.3073 0.5212 0.6404 0.034 Uiso 1 1 calc R . . C13 C 0.6972(9) 0.4139(8) 0.4568(7) 0.018(3) Uiso 1 1 d . . . C14 C 0.8261(10) 0.3009(9) 0.4154(8) 0.027(3) Uani 1 1 d . . . C15 C 0.9339(10) 0.2655(9) 0.4138(8) 0.034(4) Uani 1 1 d . . . H15A H 0.9655 0.3106 0.4061 0.041 Uiso 1 1 calc R . . H15B H 0.9457 0.2320 0.4578 0.041 Uiso 1 1 calc R . . C16 C 0.9755(12) 0.2139(10) 0.3586(9) 0.043(4) Uani 1 1 d . . . H16A H 0.9934 0.2487 0.3159 0.052 Uiso 1 1 calc R . . H16B H 0.9280 0.1875 0.3517 0.052 Uiso 1 1 calc R . . C17 C 1.0620(11) 0.1495(10) 0.3783(10) 0.052(5) Uani 1 1 d . . . H17A H 1.0994 0.1269 0.3380 0.062 Uiso 1 1 calc R . . H17B H 1.1021 0.1746 0.3960 0.062 Uiso 1 1 calc R . . C18 C 1.0341(14) 0.0814(12) 0.4312(11) 0.061(6) Uani 1 1 d . . . C30 C 0.6111(12) 0.1863(10) 0.2147(8) 0.039(4) Uani 1 1 d . . . H30A H 0.6712 0.1622 0.1875 0.047 Uiso 1 1 calc R . . H30B H 0.5687 0.1494 0.2208 0.047 Uiso 1 1 calc R . . C31 C 0.5673(11) 0.2664(10) 0.1768(8) 0.041(4) Uani 1 1 d . . . H31A H 0.6158 0.2973 0.1569 0.049 Uiso 1 1 calc R . . H31B H 0.5183 0.2985 0.2076 0.049 Uiso 1 1 calc R . . C32 C 0.5234(12) 0.2515(11) 0.1217(9) 0.048(4) Uiso 1 1 d . . . H32A H 0.5725 0.2166 0.0930 0.058 Uiso 1 1 calc R . . H32B H 0.4741 0.2216 0.1425 0.058 Uiso 1 1 calc R . . C33 C 0.4799(15) 0.3288(13) 0.0780(11) 0.071(6) Uiso 1 1 d . . . H33A H 0.4375 0.3668 0.1065 0.107 Uiso 1 1 calc R . . H33B H 0.4441 0.3162 0.0483 0.107 Uiso 1 1 calc R . . H33C H 0.5299 0.3536 0.0508 0.107 Uiso 1 1 calc R . . C34 C 0.6848(12) 0.1063(10) 0.3107(8) 0.042(4) Uiso 1 1 d . . . H34A H 0.6487 0.0670 0.3085 0.051 Uiso 1 1 calc R . . H34B H 0.7461 0.0931 0.2809 0.051 Uiso 1 1 calc R . . C35 C 0.7025(13) 0.0960(11) 0.3808(9) 0.053(5) Uiso 1 1 d . . . H35A H 0.6426 0.1150 0.4105 0.064 Uiso 1 1 calc R . . H35B H 0.7467 0.1286 0.3826 0.064 Uiso 1 1 calc R . . C36 C 0.7449(15) 0.0058(12) 0.4046(11) 0.067(6) Uiso 1 1 d . . . H36A H 0.7975 -0.0150 0.3699 0.081 Uiso 1 1 calc R . . H36B H 0.7713 0.0003 0.4462 0.081 Uiso 1 1 calc R . . C37 C 0.6755(18) -0.0442(16) 0.4180(13) 0.097(8) Uiso 1 1 d . . . H37A H 0.6288 -0.0300 0.4573 0.146 Uiso 1 1 calc R . . H37B H 0.7080 -0.1018 0.4268 0.146 Uiso 1 1 calc R . . H37C H 0.6436 -0.0341 0.3788 0.146 Uiso 1 1 calc R . . C38 C 0.5384(10) 0.2180(9) 0.3304(8) 0.036(4) Uiso 1 1 d . . . H38A H 0.5537 0.2230 0.3737 0.043 Uiso 1 1 calc R . . H38B H 0.5055 0.2728 0.3102 0.043 Uiso 1 1 calc R . . C39 C 0.4702(11) 0.1636(10) 0.3453(8) 0.042(4) Uiso 1 1 d . . . H39A H 0.4454 0.1659 0.3037 0.051 Uiso 1 1 calc R . . H39B H 0.5048 0.1068 0.3590 0.051 Uiso 1 1 calc R . . C40 C 0.3891(12) 0.1870(11) 0.3996(9) 0.047(5) Uiso 1 1 d . . . H40A H 0.4136 0.1784 0.4424 0.056 Uiso 1 1 calc R . . H40B H 0.3596 0.2457 0.3885 0.056 Uiso 1 1 calc R . . C41 C 0.3156(14) 0.1407(12) 0.4094(10) 0.063(5) Uiso 1 1 d . . . H41A H 0.2993 0.1406 0.3657 0.094 Uiso 1 1 calc R . . H41B H 0.2593 0.1664 0.4383 0.094 Uiso 1 1 calc R . . H41C H 0.3399 0.0847 0.4306 0.094 Uiso 1 1 calc R . . C42 C 0.6893(11) 0.2522(10) 0.2785(8) 0.040(4) Uiso 1 1 d . . . H42A H 0.6526 0.3066 0.2607 0.048 Uiso 1 1 calc R . . H42B H 0.6987 0.2542 0.3243 0.048 Uiso 1 1 calc R . . C43 C 0.7832(14) 0.2361(12) 0.2357(10) 0.064(6) Uiso 1 1 d . . . H43A H 0.7759 0.2250 0.1921 0.076 Uiso 1 1 calc R . . H43B H 0.8247 0.1870 0.2578 0.076 Uiso 1 1 calc R . . C44 C 0.8303(15) 0.3077(13) 0.2228(11) 0.068(6) Uiso 1 1 d . . . H44A H 0.8312 0.3224 0.2666 0.082 Uiso 1 1 calc R . . H44B H 0.8967 0.2896 0.2016 0.082 Uiso 1 1 calc R . . C45 C 0.787(2) 0.3765(17) 0.1825(14) 0.108(9) Uiso 1 1 d . . . H45A H 0.7612 0.3605 0.1487 0.161 Uiso 1 1 calc R . . H45B H 0.8335 0.4079 0.1599 0.161 Uiso 1 1 calc R . . H45C H 0.7360 0.4098 0.2102 0.161 Uiso 1 1 calc R . . C46 C 0.7765(11) 0.6512(10) 0.2767(8) 0.035(4) Uiso 1 1 d . . . H46A H 0.7676 0.6425 0.3264 0.042 Uiso 1 1 calc R . . H46B H 0.7282 0.6304 0.2638 0.042 Uiso 1 1 calc R . . C47 C 0.8729(11) 0.6009(9) 0.2516(8) 0.036(4) Uiso 1 1 d . . . H47A H 0.8839 0.6108 0.2019 0.043 Uiso 1 1 calc R . . H47B H 0.9218 0.6182 0.2671 0.043 Uiso 1 1 calc R . . C48 C 0.8820(11) 0.5114(9) 0.2764(8) 0.039(4) Uiso 1 1 d . . . H48A H 0.8683 0.5019 0.3261 0.047 Uiso 1 1 calc R . . H48B H 0.8345 0.4938 0.2594 0.047 Uiso 1 1 calc R . . C49 C 0.9781(15) 0.4607(13) 0.2544(11) 0.072(6) Uiso 1 1 d . . . H49A H 0.9875 0.4617 0.2057 0.108 Uiso 1 1 calc R . . H49B H 0.9835 0.4046 0.2777 0.108 Uiso 1 1 calc R . . H49C H 1.0261 0.4826 0.2654 0.108 Uiso 1 1 calc R . . C50 C 0.8267(11) 0.7782(10) 0.2714(7) 0.033(4) Uiso 1 1 d . . . H50A H 0.8095 0.8378 0.2570 0.039 Uiso 1 1 calc R . . H50B H 0.8902 0.7571 0.2468 0.039 Uiso 1 1 calc R . . C51 C 0.8320(11) 0.7610(10) 0.3461(8) 0.038(4) Uiso 1 1 d . . . H51A H 0.8546 0.7019 0.3609 0.045 Uiso 1 1 calc R . . H51B H 0.7688 0.7798 0.3720 0.045 Uiso 1 1 calc R . . C52 C 0.9020(11) 0.8071(10) 0.3581(8) 0.041(4) Uiso 1 1 d . . . H52A H 0.9636 0.7908 0.3295 0.049 Uiso 1 1 calc R . . H52B H 0.8771 0.8664 0.3453 0.049 Uiso 1 1 calc R . . C53 C 0.9153(12) 0.7878(10) 0.4324(8) 0.042(4) Uiso 1 1 d . . . H53A H 0.8538 0.8021 0.4608 0.063 Uiso 1 1 calc R . . H53B H 0.9567 0.8194 0.4396 0.063 Uiso 1 1 calc R . . H53C H 0.9437 0.7297 0.4442 0.063 Uiso 1 1 calc R . . C54 C 0.7706(11) 0.7599(10) 0.1739(8) 0.030(4) Uiso 1 1 d . . . H54A H 0.7588 0.8193 0.1588 0.036 Uiso 1 1 calc R . . H54B H 0.8369 0.7355 0.1559 0.036 Uiso 1 1 calc R . . C55 C 0.7062(13) 0.7274(11) 0.1445(9) 0.048(5) Uiso 1 1 d . . . H55A H 0.7261 0.6673 0.1500 0.057 Uiso 1 1 calc R . . H55B H 0.6404 0.7433 0.1673 0.057 Uiso 1 1 calc R . . C56 C 0.7137(13) 0.7636(11) 0.0709(9) 0.049(5) Uiso 1 1 d . . . H56A H 0.7811 0.7548 0.0505 0.059 Uiso 1 1 calc R . . H56B H 0.6861 0.8230 0.0663 0.059 Uiso 1 1 calc R . . C57 C 0.6602(15) 0.7242(13) 0.0311(10) 0.066(6) Uiso 1 1 d . . . H57A H 0.6929 0.6671 0.0302 0.099 Uiso 1 1 calc R . . H57B H 0.6600 0.7536 -0.0150 0.099 Uiso 1 1 calc R . . H57C H 0.5951 0.7279 0.0539 0.099 Uiso 1 1 calc R . . C58 C 0.6580(11) 0.7801(9) 0.2817(8) 0.034(4) Uiso 1 1 d . . . H58A H 0.6163 0.7482 0.2742 0.041 Uiso 1 1 calc R . . H58B H 0.6560 0.7732 0.3309 0.041 Uiso 1 1 calc R . . C59 C 0.6170(12) 0.8663(10) 0.2578(9) 0.047(4) Uiso 1 1 d . . . H59A H 0.6145 0.8739 0.2092 0.056 Uiso 1 1 calc R . . H59B H 0.6585 0.8993 0.2638 0.056 Uiso 1 1 calc R . . C60 C 0.5212(13) 0.8962(11) 0.2937(9) 0.053(5) Uiso 1 1 d . . . H60A H 0.5261 0.8962 0.3409 0.064 Uiso 1 1 calc R . . H60B H 0.4835 0.8570 0.2943 0.064 Uiso 1 1 calc R . . C61 C 0.4680(13) 0.9795(11) 0.2654(9) 0.055(5) Uiso 1 1 d . . . H61A H 0.4999 1.0201 0.2699 0.082 Uiso 1 1 calc R . . H61B H 0.4036 0.9910 0.2902 0.082 Uiso 1 1 calc R . . H61C H 0.4657 0.9817 0.2178 0.082 Uiso 1 1 calc R . . C63 C 0.5916(11) 0.4288(10) 0.8258(8) 0.034(4) Uiso 1 1 d . A 1 H63A H 0.5915 0.4857 0.8052 0.040 Uiso 1 1 calc R A 1 H63B H 0.5626 0.4075 0.7963 0.040 Uiso 1 1 calc R A 1 C64 C 0.5243(11) 0.4318(10) 0.8924(8) 0.042(4) Uiso 1 1 d . . . H64A H 0.5163 0.3767 0.9128 0.050 Uiso 1 1 calc R A 1 H64B H 0.5504 0.4523 0.9241 0.050 Uiso 1 1 calc R A 1 C65 C 0.4348(14) 0.4850(13) 0.8797(10) 0.061(6) Uiso 1 1 d . A . H65A H 0.4061 0.4602 0.8526 0.073 Uiso 1 1 calc R . . H65B H 0.4454 0.5370 0.8529 0.073 Uiso 1 1 calc R . . C66 C 0.3627(16) 0.5031(14) 0.9465(11) 0.080(7) Uiso 1 1 d . . . H66A H 0.3444 0.4531 0.9700 0.120 Uiso 1 1 calc R A . H66B H 0.3064 0.5446 0.9347 0.120 Uiso 1 1 calc R . . H66C H 0.3928 0.5227 0.9757 0.120 Uiso 1 1 calc R . . C67 C 0.7416(14) 0.3832(11) 0.8740(9) 0.050(5) Uiso 1 1 d . A 1 H67A H 0.8024 0.3424 0.8765 0.060 Uiso 1 1 calc R A 1 H67B H 0.6983 0.3729 0.9164 0.060 Uiso 1 1 calc R A 1 C68 C 0.7560(14) 0.4657(12) 0.8641(10) 0.059(5) Uiso 1 1 d . . . H68A H 0.6947 0.5043 0.8755 0.071 Uiso 1 1 calc R A 1 H68B H 0.7806 0.4822 0.8163 0.071 Uiso 1 1 calc R A 1 C69 C 0.8274(14) 0.4699(12) 0.9094(10) 0.058(5) Uiso 1 1 d . A . H69A H 0.8047 0.4499 0.9569 0.070 Uiso 1 1 calc R . . H69B H 0.8897 0.4339 0.8960 0.070 Uiso 1 1 calc R . . C70 C 0.8375(18) 0.5527(15) 0.9033(13) 0.093(8) Uiso 1 1 d . . . H70A H 0.8390 0.5791 0.8562 0.139 Uiso 1 1 calc R A . H70B H 0.8963 0.5510 0.9183 0.139 Uiso 1 1 calc R . . H70C H 0.7840 0.5835 0.9312 0.139 Uiso 1 1 calc R . . C71 C 0.753(2) 0.401(2) 0.7483(15) 0.036(8) Uiso 0.50 1 d PD A 1 C72 C 0.8568(18) 0.3542(17) 0.7387(13) 0.023(6) Uiso 0.50 1 d PD A 1 C71' C 0.721(2) 0.369(2) 0.7566(17) 0.047(10) Uiso 0.50 1 d PD B 2 C72' C 0.821(3) 0.311(3) 0.744(2) 0.071(13) Uiso 0.50 1 d PD B 2 C73' C 0.852(5) 0.305(4) 0.665(3) 0.14(3) Uiso 0.50 1 d PD B 2 C74' C 0.885(3) 0.375(3) 0.647(3) 0.060(12) Uiso 0.50 1 d PD B 2 C73 C 0.904(3) 0.383(2) 0.6666(17) 0.047(11) Uiso 0.50 1 d PD A 1 C74 C 0.857(2) 0.357(2) 0.6204(17) 0.044(8) Uiso 0.50 1 d PD A 1 C75 C 0.706(2) 0.2835(19) 0.8361(16) 0.030(7) Uiso 0.50 1 d P A 1 C76 C 0.661(2) 0.259(2) 0.7872(16) 0.037(8) Uiso 0.50 1 d P A 1 C77 C 0.656(3) 0.169(3) 0.810(2) 0.069(13) Uiso 0.50 1 d P A 1 C78 C 0.581(6) 0.149(5) 0.871(5) 0.12(3) Uiso 0.50 1 d P A 1 C75' C 0.659(2) 0.2782(17) 0.8588(15) 0.027(7) Uiso 0.50 1 d PD B 2 C76' C 0.594(3) 0.251(2) 0.8224(18) 0.049(10) Uiso 0.50 1 d PD B 2 C77' C 0.600(5) 0.162(3) 0.854(4) 0.10(3) Uiso 0.50 1 d PD B 2 C78' C 0.681(3) 0.101(3) 0.831(2) 0.083(14) Uiso 0.50 1 d PD B 2 C80 C -0.0385(12) 0.5715(10) 0.5515(8) 0.037(4) Uiso 1 1 d . . . C81 C -0.1323(12) 0.5978(11) 0.5444(9) 0.050(5) Uiso 1 1 d . . . H81A H -0.1461 0.5664 0.5149 0.075 Uiso 1 1 calc R . . H81B H -0.1463 0.6555 0.5247 0.075 Uiso 1 1 calc R . . H81C H -0.1714 0.5903 0.5886 0.075 Uiso 1 1 calc R . . C82 C 0.5398(12) 0.9400(10) 0.9392(9) 0.041(4) Uiso 1 1 d . . . C83 C 0.4398(13) 0.9592(12) 0.9305(10) 0.056(5) Uiso 1 1 d . . . H83A H 0.4116 1.0171 0.9315 0.084 Uiso 1 1 calc R . . H83B H 0.4058 0.9269 0.9669 0.084 Uiso 1 1 calc R . . H83C H 0.4358 0.9464 0.8872 0.084 Uiso 1 1 calc R . . C84 C 0.7875(17) 0.1421(14) 0.5727(11) 0.069(6) Uiso 1 1 d . . . C85 C 0.7031(15) 0.1221(14) 0.5740(11) 0.073(6) Uiso 1 1 d . . . H85A H 0.7147 0.0632 0.5765 0.110 Uiso 1 1 calc R . . H85B H 0.6767 0.1500 0.5330 0.110 Uiso 1 1 calc R . . H85C H 0.6584 0.1389 0.6134 0.110 Uiso 1 1 calc R . . C86 C 0.8718(18) 0.0171(15) 0.7165(12) 0.078(7) Uiso 1 1 d . . . C87 C 0.9569(14) 0.0405(13) 0.6981(10) 0.067(6) Uiso 1 1 d . . . H87A H 1.0094 -0.0079 0.6959 0.100 Uiso 1 1 calc R . . H87B H 0.9635 0.0705 0.7316 0.100 Uiso 1 1 calc R . . H87C H 0.9578 0.0753 0.6540 0.100 Uiso 1 1 calc R . . C96 C 1.0450(18) 0.3928(15) 0.9733(13) 0.083(7) Uiso 1 1 d . . . C97 C 0.9794(17) 0.3655(15) 1.0297(12) 0.093(8) Uiso 1 1 d . . . H97A H 1.0144 0.3259 1.0627 0.139 Uiso 1 1 calc R . . H97B H 0.9384 0.3402 1.0139 0.139 Uiso 1 1 calc R . . H97C H 0.9408 0.4121 1.0507 0.139 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 0.0222(6) 0.0179(6) 0.0156(6) -0.0030(5) -0.0062(5) -0.0070(5) Mo2 0.0207(6) 0.0183(6) 0.0150(6) -0.0002(5) -0.0048(5) -0.0094(5) Mo3 0.0262(7) 0.0170(6) 0.0187(6) -0.0005(5) -0.0069(5) -0.0107(5) Mo4 0.0162(6) 0.0186(6) 0.0176(6) -0.0049(5) 0.0010(5) -0.0045(5) Mo5 0.0176(6) 0.0183(6) 0.0179(6) 0.0009(5) -0.0015(5) -0.0042(5) Mo6 0.0153(6) 0.0173(6) 0.0213(7) -0.0040(5) -0.0013(5) -0.0011(5) Mn1 0.0109(14) 0.0092(14) 0.0114(14) -0.0038(11) -0.0037(11) -0.0048(11) Mn2 0.0126(14) 0.0149(15) 0.0126(15) -0.0024(12) -0.0033(12) -0.0095(12) O1 0.034(6) 0.045(7) 0.028(6) 0.005(5) -0.010(5) -0.026(5) O2 0.031(6) 0.020(5) 0.021(5) -0.001(4) -0.002(4) -0.015(5) O3 0.031(6) 0.015(5) 0.033(6) 0.002(4) -0.014(5) -0.011(4) O4 0.040(6) 0.013(5) 0.028(6) 0.001(4) -0.011(5) -0.008(4) O5 0.023(5) 0.020(5) 0.022(5) -0.003(4) -0.008(4) -0.008(4) O6 0.033(6) 0.015(5) 0.017(5) 0.000(4) -0.006(4) -0.001(4) O7 0.022(5) 0.015(5) 0.014(5) -0.005(4) -0.006(4) -0.010(4) O8 0.026(5) 0.039(6) 0.017(5) -0.003(4) -0.007(4) -0.010(5) O9 0.013(5) 0.018(5) 0.020(5) -0.002(4) -0.004(4) 0.002(4) O10 0.033(6) 0.030(6) 0.017(5) -0.005(4) 0.007(4) -0.008(5) O11 0.033(6) 0.031(6) 0.026(6) -0.011(5) -0.004(5) 0.002(5) O12 0.027(6) 0.034(6) 0.030(6) 0.006(5) -0.013(5) -0.015(5) O13 0.009(4) 0.026(5) 0.010(5) -0.001(4) -0.001(4) -0.006(4) O14 0.012(5) 0.026(5) 0.034(6) -0.003(4) -0.004(4) -0.002(4) O15 0.014(5) 0.021(5) 0.022(5) -0.014(4) 0.003(4) -0.007(4) O16 0.015(5) 0.034(6) 0.029(6) 0.004(5) -0.010(4) -0.007(5) O17 0.014(5) 0.025(6) 0.033(6) -0.002(4) 0.003(4) -0.001(4) O18 0.034(6) 0.040(7) 0.018(6) 0.006(5) -0.010(5) 0.002(5) O19 0.054(8) 0.053(8) 0.085(10) 0.004(7) -0.025(7) -0.019(7) O20 0.024(5) 0.024(6) 0.034(6) -0.005(5) -0.003(5) -0.004(4) O21 0.042(7) 0.032(6) 0.019(5) -0.002(4) -0.009(5) -0.007(5) O22 0.012(4) 0.013(5) 0.010(4) -0.005(4) 0.002(4) -0.008(4) O23 0.016(5) 0.015(5) 0.019(5) -0.001(4) -0.004(4) -0.003(4) O24 0.015(5) 0.030(6) 0.011(5) -0.010(4) 0.001(4) -0.012(4) O25 0.017(5) 0.021(5) 0.022(5) -0.015(4) -0.002(4) -0.005(4) O26 0.021(6) 0.071(9) 0.079(9) -0.057(8) 0.011(6) -0.017(6) O29 0.021(5) 0.033(6) 0.045(7) -0.014(5) -0.006(5) -0.004(5) N1 0.020(6) 0.029(7) 0.035(7) -0.020(6) 0.003(5) -0.010(5) N2 0.010(6) 0.028(7) 0.031(7) -0.015(5) 0.000(5) -0.001(5) N3 0.030(7) 0.040(8) 0.040(8) -0.018(6) -0.006(6) 0.001(6) N4 0.016(6) 0.036(8) 0.042(9) 0.013(5) -0.003(6) -0.015(6) C5 0.032(9) 0.046(10) 0.027(9) -0.013(7) -0.014(7) -0.011(8) C6 0.024(9) 0.077(14) 0.066(13) -0.055(11) -0.006(8) -0.008(9) C7 0.018(7) 0.034(8) 0.029(8) -0.017(7) -0.008(6) -0.006(6) C8 0.032(9) 0.061(12) 0.057(11) -0.041(9) -0.007(8) -0.018(8) C9 0.020(8) 0.060(11) 0.046(10) -0.035(9) 0.000(7) -0.011(8) C11 0.026(7) 0.009(6) 0.025(8) -0.008(5) 0.000(6) 0.005(6) C12 0.012(7) 0.041(9) 0.023(8) -0.010(7) 0.006(6) 0.005(6) C14 0.017(7) 0.033(9) 0.036(9) -0.013(7) 0.007(6) -0.017(7) C15 0.023(8) 0.025(8) 0.047(10) -0.009(7) -0.002(7) 0.005(7) C16 0.036(9) 0.039(10) 0.049(11) -0.018(8) 0.000(8) 0.002(8) C17 0.016(8) 0.041(11) 0.076(14) 0.004(9) -0.004(8) 0.016(7) C18 0.043(12) 0.043(11) 0.095(17) -0.025(11) -0.012(11) 0.002(9) C30 0.051(11) 0.039(10) 0.039(10) -0.023(8) -0.005(8) -0.020(8) C31 0.038(9) 0.048(10) 0.042(10) -0.013(8) -0.001(8) -0.019(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O8 1.699(9) . ? Mo1 O3 1.730(9) . ? Mo1 O7 1.902(9) . ? Mo1 O5 1.903(9) . ? Mo1 O9 2.328(9) . ? Mo1 O6 2.400(9) . ? Mo2 O10 1.690(9) . ? Mo2 O12 1.698(10) . ? Mo2 O2 1.914(10) . ? Mo2 O7 1.921(8) . ? Mo2 O9 2.309(9) . ? Mo2 O13 2.386(8) . ? Mo3 O4 1.670(9) . ? Mo3 O1 1.715(10) . ? Mo3 O2 1.918(9) 2_666 ? Mo3 O5 1.928(9) . ? Mo3 O6 2.319(9) . ? Mo3 O13 2.390(9) 2_666 ? Mo4 O21 1.687(9) . ? Mo4 O20 1.689(10) . ? Mo4 O23 1.901(9) . ? Mo4 O15 1.902(9) . ? Mo4 O22 2.338(8) . ? Mo4 O24 2.354(9) . ? Mo5 O18 1.715(10) . ? Mo5 O17 1.727(10) . ? Mo5 O16 1.914(9) . ? Mo5 O23 1.926(9) 2_757 ? Mo5 O25 2.299(9) . ? Mo5 O24 2.432(9) 2_757 ? Mo6 O11 1.691(10) . ? Mo6 O14 1.703(9) . ? Mo6 O16 1.923(10) . ? Mo6 O15 1.924(9) . ? Mo6 O25 2.318(9) . ? Mo6 O22 2.432(8) . ? Mn1 O13 1.911(9) . ? Mn1 O13 1.911(9) 2_666 ? Mn1 O6 1.980(10) . ? Mn1 O6 1.980(10) 2_666 ? Mn1 O9 2.060(9) . ? Mn1 O9 2.060(9) 2_666 ? Mn2 O24 1.920(8) 2_757 ? Mn2 O24 1.920(8) . ? Mn2 O22 1.965(8) . ? Mn2 O22 1.965(8) 2_757 ? Mn2 O25 2.107(9) 2_757 ? Mn2 O25 2.107(9) . ? O2 Mo3 1.918(9) 2_666 ? O6 C10 1.437(15) . ? O9 C12 1.465(15) . ? O13 C11 1.474(15) . ? O13 Mo3 2.390(9) 2_666 ? O19 C18 1.21(2) . ? O22 C1 1.423(15) . ? O23 Mo5 1.926(9) 2_757 ? O24 C3 1.449(15) 2_757 ? O24 Mo5 2.432(9) 2_757 ? O25 C2 1.403(14) . ? O26 C5 1.222(18) . ? O27 C9 1.218(18) . ? O28 C9 1.316(18) . ? O29 C14 1.217(16) . ? O30 C18 1.31(2) . ? N1 C5 1.364(18) . ? N1 C4 1.481(17) . ? N2 C14 1.340(18) . ? N2 C13 1.449(17) . ? N3 C42 1.52(2) . ? N3 C38 1.521(18) . ? N3 C34 1.52(2) . ? N3 C30 1.544(19) . ? N4 C50 1.497(19) . ? N4 C58 1.518(19) . ? N4 C46 1.53(2) . ? N4 C54 1.537(19) . ? N5 C67 1.37(3) . ? N5 C71 1.54(3) . ? N5 C75 1.59(4) . ? N5 C63 1.66(3) . ? N5' C75' 1.48(3) . ? N5' C71' 1.56(3) . ? N6 C80 1.16(2) . ? N7 C82 1.12(2) . ? N8 C84 1.19(3) . ? N9 C86 1.20(3) . ? N10 C96 1.15(3) . ? C1 C4 1.524(18) . ? C2 C4 1.567(18) 2_757 ? C3 O24 1.449(15) 2_757 ? C3 C4 1.557(18) . ? C4 C2 1.567(18) 2_757 ? C5 C6 1.50(2) . ? C6 C7 1.521(19) . ? C7 C8 1.532(18) . ? C8 C9 1.456(19) . ? C10 C13 1.562(18) . ? C11 C13 1.523(18) . ? C12 C13 1.542(19) 2_666 ? C13 C12 1.542(19) 2_666 ? C14 C15 1.55(2) . ? C15 C16 1.52(2) . ? C16 C17 1.52(2) . ? C17 C18 1.52(3) . ? C30 C31 1.49(2) . ? C31 C32 1.52(2) . ? C32 C33 1.51(3) . ? C34 C35 1.49(2) . ? C35 C36 1.53(3) . ? C36 C37 1.48(3) . ? C38 C39 1.52(2) . ? C39 C40 1.50(2) . ? C40 C41 1.49(2) . ? C42 C43 1.48(2) . ? C43 C44 1.54(3) . ? C44 C45 1.38(3) . ? C46 C47 1.51(2) . ? C47 C48 1.51(2) . ? C48 C49 1.50(2) . ? C50 C51 1.52(2) . ? C51 C52 1.56(2) . ? C52 C53 1.54(2) . ? C54 C55 1.51(2) . ? C55 C56 1.51(2) . ? C56 C57 1.61(2) . ? C58 C59 1.47(2) . ? C59 C60 1.48(2) . ? C60 C61 1.51(2) . ? C63 C64 1.53(2) . ? C64 C65 1.44(2) . ? C65 C66 1.59(3) . ? C67 C68 1.47(3) . ? C68 C69 1.58(3) . ? C69 C70 1.46(3) . ? C71 C72 1.53(3) . ? C72 C73 1.55(3) . ? C71' C72' 1.56(4) . ? C72' C73' 1.61(4) . ? C73' C74' 1.38(4) . ? C73 C74 1.51(4) . ? C75 C76 1.50(4) . ? C76 C77 1.55(5) . ? C77 C78 1.55(10) . ? C75' C76' 1.55(3) . ? C76' C77' 1.54(4) . ? C77' C78' 1.44(5) . ? C80 C81 1.38(2) . ? C82 C83 1.48(2) . ? C84 C85 1.39(3) . ? C86 C87 1.39(3) . ? C96 C97 1.45(3) . ? 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 O8 Mo1 O3 104.1(5) . . ? O8 Mo1 O7 103.1(4) . . ? O3 Mo1 O7 98.3(4) . . ? O8 Mo1 O5 100.2(4) . . ? O3 Mo1 O5 101.6(4) . . ? O7 Mo1 O5 144.4(4) . . ? O8 Mo1 O9 92.6(4) . . ? O3 Mo1 O9 162.0(4) . . ? O7 Mo1 O9 70.7(3) . . ? O5 Mo1 O9 81.9(3) . . ? O8 Mo1 O6 162.2(4) . . ? O3 Mo1 O6 92.4(4) . . ? O7 Mo1 O6 80.6(3) . . ? O5 Mo1 O6 69.5(3) . . ? O9 Mo1 O6 72.0(3) . . ? O10 Mo2 O12 104.2(5) . . ? O10 Mo2 O2 100.6(5) . . ? O12 Mo2 O2 101.9(4) . . ? O10 Mo2 O7 101.4(4) . . ? O12 Mo2 O7 98.1(4) . . ? O2 Mo2 O7 145.4(4) . . ? O10 Mo2 O9 95.7(4) . . ? O12 Mo2 O9 158.9(4) . . ? O2 Mo2 O9 80.7(4) . . ? O7 Mo2 O9 70.8(3) . . ? O10 Mo2 O13 165.5(4) . . ? O12 Mo2 O13 89.3(4) . . ? O2 Mo2 O13 71.1(3) . . ? O7 Mo2 O13 81.4(3) . . ? O9 Mo2 O13 71.6(3) . . ? O4 Mo3 O1 106.4(5) . . ? O4 Mo3 O2 101.5(4) . 2_666 ? O1 Mo3 O2 98.6(5) . 2_666 ? O4 Mo3 O5 98.7(4) . . ? O1 Mo3 O5 103.4(4) . . ? O2 Mo3 O5 144.4(4) 2_666 . ? O4 Mo3 O6 159.7(4) . . ? O1 Mo3 O6 93.2(4) . . ? O2 Mo3 O6 80.2(4) 2_666 . ? O5 Mo3 O6 71.0(4) . . ? O4 Mo3 O13 91.9(4) . 2_666 ? O1 Mo3 O13 160.6(4) . 2_666 ? O2 Mo3 O13 70.9(3) 2_666 2_666 ? O5 Mo3 O13 79.4(3) . 2_666 ? O6 Mo3 O13 69.4(3) . 2_666 ? O21 Mo4 O20 103.5(5) . . ? O21 Mo4 O23 101.6(4) . . ? O20 Mo4 O23 98.5(4) . . ? O21 Mo4 O15 99.8(4) . . ? O20 Mo4 O15 101.3(4) . . ? O23 Mo4 O15 146.4(4) . . ? O21 Mo4 O22 161.4(4) . . ? O20 Mo4 O22 94.6(4) . . ? O23 Mo4 O22 79.4(3) . . ? O15 Mo4 O22 72.1(3) . . ? O21 Mo4 O24 92.6(4) . . ? O20 Mo4 O24 162.8(4) . . ? O23 Mo4 O24 72.0(3) . . ? O15 Mo4 O24 81.5(3) . . ? O22 Mo4 O24 69.8(3) . . ? O18 Mo5 O17 106.1(5) . . ? O18 Mo5 O16 97.6(5) . . ? O17 Mo5 O16 103.4(4) . . ? O18 Mo5 O23 99.7(4) . 2_757 ? O17 Mo5 O23 100.2(4) . 2_757 ? O16 Mo5 O23 145.5(4) . 2_757 ? O18 Mo5 O25 159.7(4) . . ? O17 Mo5 O25 93.4(4) . . ? O16 Mo5 O25 71.8(4) . . ? O23 Mo5 O25 82.1(3) 2_757 . ? O18 Mo5 O24 89.0(4) . 2_757 ? O17 Mo5 O24 163.4(4) . 2_757 ? O16 Mo5 O24 80.9(4) . 2_757 ? O23 Mo5 O24 69.8(3) 2_757 2_757 ? O25 Mo5 O24 72.6(3) . 2_757 ? O11 Mo6 O14 105.0(5) . . ? O11 Mo6 O16 102.7(5) . . ? O14 Mo6 O16 96.0(4) . . ? O11 Mo6 O15 101.2(4) . . ? O14 Mo6 O15 101.7(4) . . ? O16 Mo6 O15 145.3(4) . . ? O11 Mo6 O25 94.6(4) . . ? O14 Mo6 O25 158.7(4) . . ? O16 Mo6 O25 71.2(3) . . ? O15 Mo6 O25 82.1(3) . . ? O11 Mo6 O22 164.9(4) . . ? O14 Mo6 O22 88.9(4) . . ? O16 Mo6 O22 81.2(4) . . ? O15 Mo6 O22 69.6(3) . . ? O25 Mo6 O22 72.6(3) . . ? O13 Mn1 O13 180.0(5) . 2_666 ? O13 Mn1 O6 92.9(4) . . ? O13 Mn1 O6 87.1(4) 2_666 . ? O13 Mn1 O6 87.1(4) . 2_666 ? O13 Mn1 O6 92.9(4) 2_666 2_666 ? O6 Mn1 O6 180.0(5) . 2_666 ? O13 Mn1 O9 87.4(3) . . ? O13 Mn1 O9 92.6(3) 2_666 . ? O6 Mn1 O9 87.0(4) . . ? O6 Mn1 O9 93.0(4) 2_666 . ? O13 Mn1 O9 92.6(3) . 2_666 ? O13 Mn1 O9 87.4(3) 2_666 2_666 ? O6 Mn1 O9 93.0(4) . 2_666 ? O6 Mn1 O9 87.0(4) 2_666 2_666 ? O9 Mn1 O9 180.000(1) . 2_666 ? O24 Mn2 O24 180.000(1) 2_757 . ? O24 Mn2 O22 92.5(3) 2_757 . ? O24 Mn2 O22 87.5(3) . . ? O24 Mn2 O22 87.5(3) 2_757 2_757 ? O24 Mn2 O22 92.5(3) . 2_757 ? O22 Mn2 O22 180.0(5) . 2_757 ? O24 Mn2 O25 91.9(4) 2_757 2_757 ? O24 Mn2 O25 88.1(4) . 2_757 ? O22 Mn2 O25 92.6(3) . 2_757 ? O22 Mn2 O25 87.4(3) 2_757 2_757 ? O24 Mn2 O25 88.1(4) 2_757 . ? O24 Mn2 O25 91.9(4) . . ? O22 Mn2 O25 87.4(3) . . ? O22 Mn2 O25 92.6(3) 2_757 . ? O25 Mn2 O25 180.0(5) 2_757 . ? Mo2 O2 Mo3 122.3(5) . 2_666 ? Mo1 O5 Mo3 123.0(5) . . ? C10 O6 Mn1 115.8(7) . . ? C10 O6 Mo3 119.0(8) . . ? Mn1 O6 Mo3 101.9(4) . . ? C10 O6 Mo1 123.9(8) . . ? Mn1 O6 Mo1 100.5(4) . . ? Mo3 O6 Mo1 91.0(3) . . ? Mo1 O7 Mo2 121.8(5) . . ? C12 O9 Mn1 114.9(8) . . ? C12 O9 Mo2 122.8(8) . . ? Mn1 O9 Mo2 99.5(4) . . ? C12 O9 Mo1 121.9(8) . . ? Mn1 O9 Mo1 100.5(4) . . ? Mo2 O9 Mo1 92.2(3) . . ? C11 O13 Mn1 117.9(7) . . ? C11 O13 Mo2 120.1(7) . . ? Mn1 O13 Mo2 101.4(4) . . ? C11 O13 Mo3 121.2(7) . 2_666 ? Mn1 O13 Mo3 101.6(3) . 2_666 ? Mo2 O13 Mo3 89.3(3) . 2_666 ? Mo4 O15 Mo6 123.8(4) . . ? Mo5 O16 Mo6 120.5(5) . . ? C1 O22 Mn2 115.6(7) . . ? C1 O22 Mo4 120.4(7) . . ? Mn2 O22 Mo4 100.9(3) . . ? C1 O22 Mo6 124.4(8) . . ? Mn2 O22 Mo6 100.2(3) . . ? Mo4 O22 Mo6 90.0(3) . . ? Mo4 O23 Mo5 123.0(5) . 2_757 ? C3 O24 Mn2 119.6(7) 2_757 . ? C3 O24 Mo4 118.2(7) 2_757 . ? Mn2 O24 Mo4 101.8(4) . . ? C3 O24 Mo5 122.1(7) 2_757 2_757 ? Mn2 O24 Mo5 100.2(3) . 2_757 ? Mo4 O24 Mo5 89.3(3) . 2_757 ? C2 O25 Mn2 113.9(7) . . ? C2 O25 Mo5 122.6(7) . . ? Mn2 O25 Mo5 99.1(3) . . ? C2 O25 Mo6 123.9(7) . . ? Mn2 O25 Mo6 99.8(3) . . ? Mo5 O25 Mo6 92.4(3) . . ? C5 N1 C4 126.0(12) . . ? C14 N2 C13 126.9(12) . . ? C42 N3 C38 108.1(11) . . ? C42 N3 C34 110.3(12) . . ? C38 N3 C34 111.6(12) . . ? C42 N3 C30 111.3(12) . . ? C38 N3 C30 110.3(12) . . ? C34 N3 C30 105.3(11) . . ? C50 N4 C58 110.4(11) . . ? C50 N4 C46 110.8(12) . . ? C58 N4 C46 106.9(12) . . ? C50 N4 C54 106.8(12) . . ? C58 N4 C54 111.3(12) . . ? C46 N4 C54 110.7(10) . . ? C67 N5 C71 119(2) . . ? C67 N5 C75 99.6(18) . . ? C71 N5 C75 111(2) . . ? C67 N5 C63 110.7(16) . . ? C71 N5 C63 107.9(17) . . ? C75 N5 C63 107.6(19) . . ? C75' N5' C71' 112(3) . . ? O22 C1 C4 115.3(11) . . ? O25 C2 C4 114.7(10) . 2_757 ? O24 C3 C4 110.6(10) 2_757 . ? N1 C4 C1 103.5(10) . . ? N1 C4 C3 108.2(11) . . ? C1 C4 C3 114.6(11) . . ? N1 C4 C2 107.4(11) . 2_757 ? C1 C4 C2 110.7(11) . 2_757 ? C3 C4 C2 111.8(11) . 2_757 ? O26 C5 N1 124.7(14) . . ? O26 C5 C6 121.8(14) . . ? N1 C5 C6 113.4(13) . . ? C5 C6 C7 115.9(13) . . ? C6 C7 C8 110.6(12) . . ? C9 C8 C7 113.8(13) . . ? O27 C9 O28 120.4(14) . . ? O27 C9 C8 127.4(15) . . ? O28 C9 C8 112.1(13) . . ? O6 C10 C13 114.1(10) . . ? O13 C11 C13 112.3(10) . . ? O9 C12 C13 112.6(10) . 2_666 ? N2 C13 C11 106.0(11) . . ? N2 C13 C12 106.7(10) . 2_666 ? C11 C13 C12 114.0(11) . 2_666 ? N2 C13 C10 105.5(10) . . ? C11 C13 C10 112.0(11) . . ? C12 C13 C10 112.0(11) 2_666 . ? O29 C14 N2 123.5(13) . . ? O29 C14 C15 123.0(13) . . ? N2 C14 C15 113.0(12) . . ? C16 C15 C14 111.5(13) . . ? C15 C16 C17 109.7(15) . . ? C18 C17 C16 111.1(14) . . ? O19 C18 O30 126(2) . . ? O19 C18 C17 122.1(19) . . ? O30 C18 C17 111.8(17) . . ? C31 C30 N3 113.7(12) . . ? C30 C31 C32 108.5(13) . . ? C33 C32 C31 113.2(16) . . ? C35 C34 N3 114.0(14) . . ? C34 C35 C36 108.8(15) . . ? C37 C36 C35 113.0(19) . . ? C39 C38 N3 116.9(13) . . ? C40 C39 C38 112.9(14) . . ? C41 C40 C39 113.7(15) . . ? C43 C42 N3 116.3(14) . . ? C42 C43 C44 112.7(16) . . ? C45 C44 C43 115(2) . . ? C47 C46 N4 116.1(13) . . ? C48 C47 C46 111.9(13) . . ? C49 C48 C47 112.9(15) . . ? N4 C50 C51 115.3(13) . . ? C50 C51 C52 107.9(13) . . ? C53 C52 C51 110.5(13) . . ? C55 C54 N4 113.9(13) . . ? C56 C55 C54 106.7(14) . . ? C55 C56 C57 111.8(15) . . ? C59 C58 N4 118.2(14) . . ? C58 C59 C60 112.7(15) . . ? C59 C60 C61 116.3(16) . . ? C64 C63 N5 122.8(14) . . ? C65 C64 C63 108.6(15) . . ? C64 C65 C66 113.5(17) . . ? N5 C67 C68 107.8(17) . . ? C67 C68 C69 111.2(16) . . ? C70 C69 C68 111.6(18) . . ? C72 C71 N5 111(2) . . ? C71 C72 C73 109(2) . . ? N5' C71' C72' 116(3) . . ? C71' C72' C73' 110(4) . . ? C74' C73' C72' 96(4) . . ? C74 C73 C72 105(3) . . ? C76 C75 N5 113(2) . . ? C75 C76 C77 110(3) . . ? C76 C77 C78 118(5) . . ? N5' C75' C76' 113(3) . . ? C77' C76' C75' 104(4) . . ? C78' C77' C76' 119(5) . . ? N6 C80 C81 176.0(19) . . ? N7 C82 C83 176(2) . . ? N8 C84 C85 177(3) . . ? N9 C86 C87 171(3) . . ? N10 C96 C97 175(3) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.59 _refine_diff_density_min -1.16 _refine_diff_density_rms 0.19 data_mh242 _database_code_depnum_ccdc_archive 'CCDC 909167' #TrackingRef 'MnMo6-6-DMF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H161 Mn Mo6 N8 O33' _chemical_formula_weight 2357.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.8569(2) _cell_length_b 27.1013(3) _cell_length_c 21.2905(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.1110(10) _cell_angle_gamma 90.00 _cell_volume 10303.42(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 45480 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 26.0 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4880 _exptl_absorpt_coefficient_mu 0.902 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7863 _exptl_absorpt_correction_T_max 0.9152 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Oxford Gemini Ultra A CCD' _diffrn_measurement_method '\w & \p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 163257 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 26.00 _reflns_number_total 20213 _reflns_number_gt 15887 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics diamond3 _computing_publication_material WinGX _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^ > 2\s(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^)+(0.0408P)^2^+21.6133P] 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 none _refine_ls_number_reflns 20213 _refine_ls_number_parameters 1072 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0891 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.038 _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 0.116229(18) 0.909316(11) 0.046802(14) 0.02493(8) Uani 1 1 d . . . Mo2 Mo 0.100129(18) 0.938009(11) -0.106213(14) 0.02394(8) Uani 1 1 d . . . Mo3 Mo 0.014831(18) 0.971265(12) 0.153381(14) 0.02592(8) Uani 1 1 d . . . Mo4 Mo 0.918882(18) 0.588387(12) 0.911277(16) 0.02883(8) Uani 1 1 d . . . Mo5 Mo 1.105844(17) 0.582937(11) 0.926008(15) 0.02572(8) Uani 1 1 d . . . Mo6 Mo 0.812758(17) 0.503717(12) 0.984246(15) 0.02633(8) Uani 1 1 d . . . Mn1 Mn 0.0000 1.0000 0.0000 0.01901(15) Uani 1 2 d S . . Mn2 Mn 1.0000 0.5000 1.0000 0.01989(15) Uani 1 2 d S . . O1 O 0.08406(14) 1.00315(9) -0.13810(11) 0.0255(5) Uani 1 1 d . . . O2 O 0.19583(15) 0.93636(10) -0.11161(13) 0.0343(6) Uani 1 1 d . . . O3 O 0.06780(16) 0.90324(9) -0.16682(12) 0.0344(6) Uani 1 1 d . . . O4 O 0.08247(14) 0.89425(8) -0.03739(11) 0.0248(5) Uani 1 1 d . . . O5 O 0.21057(15) 0.91290(10) 0.03603(13) 0.0356(6) Uani 1 1 d . . . O6 O 0.10383(13) 0.98462(8) -0.01238(11) 0.0215(5) Uani 1 1 d . . . O7 O -0.02085(13) 0.96351(8) -0.07639(11) 0.0232(5) Uani 1 1 d . . . O8 O -0.00617(13) 0.93588(8) 0.05541(11) 0.0227(5) Uani 1 1 d . . . O9 O 0.10133(16) 0.85344(10) 0.08142(12) 0.0358(6) Uani 1 1 d . . . O10 O 0.10968(14) 0.95474(9) 0.11581(11) 0.0275(6) Uani 1 1 d . . . O11 O -0.00859(17) 0.91989(11) 0.19503(13) 0.0409(7) Uani 1 1 d . . . O12 O 0.04809(16) 1.01172(11) 0.20792(12) 0.0403(7) Uani 1 1 d . . . O13 O 1.16452(13) 0.52429(9) 0.93440(12) 0.0263(5) Uani 1 1 d . . . O14 O 1.11728(16) 0.59432(10) 0.84811(13) 0.0365(6) Uani 1 1 d . . . O15 O 1.16078(14) 0.62533(10) 0.96401(13) 0.0340(6) Uani 1 1 d . . . O16 O 0.93004(17) 0.59574(11) 0.83256(14) 0.0431(7) Uani 1 1 d . . . O17 O 1.01068(14) 0.61370(9) 0.94396(12) 0.0279(6) Uani 1 1 d . . . O18 O 1.07561(13) 0.54540(9) 1.02382(11) 0.0237(5) Uani 1 1 d . . . O19 O 1.01145(13) 0.52484(9) 0.91184(11) 0.0250(5) Uani 1 1 d . . . O20 O 0.85409(13) 0.53208(10) 0.90895(12) 0.0287(6) Uani 1 1 d . . . O21 O 0.91570(13) 0.55095(9) 1.01122(11) 0.0263(5) Uani 1 1 d . . . O22 O 0.76517(15) 0.45629(11) 0.95000(14) 0.0397(7) Uani 1 1 d . . . O23 O 0.74697(15) 0.54575(11) 1.00626(14) 0.0406(7) Uani 1 1 d . . . O24 O 0.85945(15) 0.63483(10) 0.93444(15) 0.0420(7) Uani 1 1 d . . . O25 O 0.13118(15) 1.17562(10) 0.05866(14) 0.0393(7) Uani 1 1 d . . . O26 O 0.21679(17) 1.28003(11) 0.04825(15) 0.0464(8) Uani 1 1 d . . . H26 H 0.1879 1.3032 0.0581 0.070 Uiso 1 1 calc R . . O27 O 0.21222(19) 1.26426(12) 0.15126(16) 0.0516(8) Uani 1 1 d . . . O28 O 1.11899(16) 0.42176(11) 0.78690(13) 0.0409(7) Uani 1 1 d . . . O29 O 1.15976(18) 0.41401(12) 0.63723(15) 0.0492(8) Uani 1 1 d . . . H29 H 1.2061 0.4179 0.6325 0.074 Uiso 1 1 calc R . . O30 O 1.19643(18) 0.34472(13) 0.68473(15) 0.0513(8) Uani 1 1 d . . . O31 O 0.4972(5) 0.8517(4) 0.0060(4) 0.092(3) Uiso 0.50 1 d P . . O32 O 0.8784(2) 0.33163(15) 0.8416(2) 0.0856(14) Uani 1 1 d . . . O33 O 0.3331(2) 0.06775(14) 0.9840(2) 0.0714(11) Uani 1 1 d . . . N1 N 0.18578(17) 1.10760(11) 0.01564(15) 0.0280(7) Uani 1 1 d . . . H1 H 0.2293 1.0954 0.0041 0.034 Uiso 1 1 calc R . . N2 N 1.01214(17) 0.39933(12) 0.83694(15) 0.0312(7) Uani 1 1 d . . . H2 H 0.9730 0.3797 0.8344 0.037 Uiso 1 1 calc R . . N3 N 0.7896(2) 0.11131(14) 0.73338(17) 0.0466(10) Uani 1 1 d . . . N4 N 0.9052(2) 0.24494(12) 0.09668(19) 0.0468(10) Uani 1 1 d . D . N5 N 0.16359(17) -0.00562(12) 0.68108(14) 0.0319(7) Uani 1 1 d . . . N6 N 0.5531(5) 0.7996(3) 0.0718(4) 0.060(2) Uiso 0.50 1 d P . . N7 N 0.7563(2) 0.32731(17) 0.8675(2) 0.0628(12) Uani 1 1 d . . . N8 N 0.3748(3) -0.00375(17) 1.0257(2) 0.0736(14) Uani 1 1 d . . . C1 C 0.1209(2) 1.07443(13) 0.01103(17) 0.0251(8) Uani 1 1 d . . . C2 C 0.1566(2) 1.02437(13) -0.00648(18) 0.0269(8) Uani 1 1 d . . . H2A H 0.1835 1.0281 -0.0468 0.032 Uiso 1 1 calc R . . H2B H 0.1939 1.0155 0.0260 0.032 Uiso 1 1 calc R . . C3 C -0.0823(2) 0.92858(13) -0.07542(17) 0.0275(8) Uani 1 1 d . . . H3A H -0.0631 0.8955 -0.0868 0.033 Uiso 1 1 calc R . . H3B H -0.1197 0.9383 -0.1075 0.033 Uiso 1 1 calc R . . C4 C -0.0695(2) 0.90523(13) 0.04141(17) 0.0256(8) Uani 1 1 d . . . H4A H -0.0995 0.9011 0.0801 0.031 Uiso 1 1 calc R . . H4B H -0.0513 0.8722 0.0287 0.031 Uiso 1 1 calc R . . C5 C 0.1855(2) 1.15485(14) 0.03581(19) 0.0324(9) Uani 1 1 d . . . C6 C 0.2593(2) 1.18192(15) 0.0261(2) 0.0395(10) Uani 1 1 d . . . H6A H 0.2536 1.2053 -0.0093 0.047 Uiso 1 1 calc R . . H6B H 0.2983 1.1577 0.0144 0.047 Uiso 1 1 calc R . . C7 C 0.2855(2) 1.21046(16) 0.0843(2) 0.0432(11) Uani 1 1 d . . . C8 C 0.2329(2) 1.25330(15) 0.0993(2) 0.0394(10) Uani 1 1 d . . . C9 C 0.2921(3) 1.17646(19) 0.1404(3) 0.0650(15) Uani 1 1 d . . . H9A H 0.3161 1.1941 0.1752 0.097 Uiso 1 1 calc R . . H9B H 0.3224 1.1477 0.1291 0.097 Uiso 1 1 calc R . . H9C H 0.2420 1.1656 0.1532 0.097 Uiso 1 1 calc R . . C10 C 0.3619(3) 1.23368(19) 0.0691(3) 0.0615(15) Uani 1 1 d . . . H10A H 0.3567 1.2560 0.0331 0.092 Uiso 1 1 calc R . . H10B H 0.3979 1.2076 0.0589 0.092 Uiso 1 1 calc R . . H10C H 0.3800 1.2523 0.1056 0.092 Uiso 1 1 calc R . . C11 C 1.0136(2) 0.43476(13) 0.88961(17) 0.0266(8) Uani 1 1 d . . . C12 C 1.0152(2) 0.48787(14) 0.86318(18) 0.0292(8) Uani 1 1 d . . . H12A H 1.0618 0.4926 0.8388 0.035 Uiso 1 1 calc R . . H12B H 0.9724 0.4923 0.8341 0.035 Uiso 1 1 calc R . . C13 C 1.0612(2) 0.57606(14) 1.07720(18) 0.0293(8) Uani 1 1 d . . . H13A H 1.0614 0.6110 1.0635 0.035 Uiso 1 1 calc R . . H13B H 1.1025 0.5718 1.1078 0.035 Uiso 1 1 calc R . . C14 C 0.9186(2) 0.57828(14) 1.06897(17) 0.0280(8) Uani 1 1 d . . . H14A H 0.8722 0.5719 1.0930 0.034 Uiso 1 1 calc R . . H14B H 0.9202 0.6140 1.0591 0.034 Uiso 1 1 calc R . . C15 C 1.0646(2) 0.39413(15) 0.79262(19) 0.0358(9) Uani 1 1 d . . . C16 C 1.0539(3) 0.34949(17) 0.7499(2) 0.0468(11) Uani 1 1 d . . . H16A H 1.0902 0.3235 0.7620 0.056 Uiso 1 1 calc R . . H16B H 1.0029 0.3361 0.7560 0.056 Uiso 1 1 calc R . . C17 C 1.0647(3) 0.36220(19) 0.6811(2) 0.0485(12) Uani 1 1 d . . . C18 C 1.1474(3) 0.37304(17) 0.66931(19) 0.0408(10) Uani 1 1 d . . . C19 C 1.0460(3) 0.3155(2) 0.6424(3) 0.0742(19) Uani 1 1 d . . . H19A H 1.0512 0.3228 0.5975 0.111 Uiso 1 1 calc R . . H19B H 0.9944 0.3052 0.6511 0.111 Uiso 1 1 calc R . . H19C H 1.0804 0.2889 0.6540 0.111 Uiso 1 1 calc R . . C20 C 1.0131(3) 0.4047(2) 0.6619(3) 0.0671(16) Uani 1 1 d . . . H20A H 1.0304 0.4353 0.6817 0.101 Uiso 1 1 calc R . . H20B H 0.9619 0.3976 0.6756 0.101 Uiso 1 1 calc R . . H20C H 1.0140 0.4085 0.6161 0.101 Uiso 1 1 calc R . . C21 C 0.8551(3) 0.13793(17) 0.7643(2) 0.0482(12) Uani 1 1 d . A . H21A H 0.8518 0.1328 0.8103 0.058 Uiso 1 1 calc R . . H21B H 0.9021 0.1223 0.7498 0.058 Uiso 1 1 calc R . . C22 C 0.8602(3) 0.1930(2) 0.7520(3) 0.0704(17) Uani 1 1 d . . . H22A H 0.8163 0.2097 0.7708 0.084 Uiso 1 1 calc R A . H22B H 0.8592 0.1990 0.7062 0.084 Uiso 1 1 calc R . . C23 C 0.9316(3) 0.2147(2) 0.7796(3) 0.0619(14) Uani 1 1 d . A . H23A H 0.9275 0.2511 0.7797 0.074 Uiso 1 1 calc R . . H23B H 0.9368 0.2036 0.8237 0.074 Uiso 1 1 calc R . . C24 C 1.0000(4) 0.2003(2) 0.7443(3) 0.0802(18) Uani 1 1 d . . . H24A H 1.0085 0.1648 0.7491 0.120 Uiso 1 1 calc R A . H24B H 1.0432 0.2185 0.7609 0.120 Uiso 1 1 calc R . . H24C H 0.9933 0.2082 0.6998 0.120 Uiso 1 1 calc R . . C25 C 0.7918(3) 0.11635(19) 0.6628(2) 0.0504(12) Uani 1 1 d . A . H25A H 0.7468 0.1000 0.6453 0.060 Uiso 1 1 calc R . . H25B H 0.7882 0.1519 0.6523 0.060 Uiso 1 1 calc R . . C26 C 0.8596(4) 0.0956(2) 0.6304(3) 0.0779(18) Uani 1 1 d . . . H26A H 0.8536 0.0595 0.6252 0.093 Uiso 1 1 calc R A . H26B H 0.9046 0.1015 0.6566 0.093 Uiso 1 1 calc R . . C27 C 0.8704(3) 0.1195(2) 0.5659(3) 0.0638(15) Uani 1 1 d . A . H27A H 0.8228 0.1172 0.5421 0.077 Uiso 1 1 calc R . . H27B H 0.8818 0.1550 0.5719 0.077 Uiso 1 1 calc R . . C28 C 0.9301(4) 0.0971(3) 0.5288(4) 0.104(2) Uiso 1 1 d . . . H28A H 0.9768 0.0974 0.5530 0.155 Uiso 1 1 calc R A . H28B H 0.9369 0.1159 0.4899 0.155 Uiso 1 1 calc R . . H28C H 0.9166 0.0630 0.5185 0.155 Uiso 1 1 calc R . . C29 C 0.7964(3) 0.05728(18) 0.7527(3) 0.0608(15) Uani 1 1 d . A . H29A H 0.8441 0.0442 0.7359 0.073 Uiso 1 1 calc R . . H29B H 0.7993 0.0556 0.7991 0.073 Uiso 1 1 calc R . . C30 C 0.7334(4) 0.02408(19) 0.7310(3) 0.0734(18) Uani 1 1 d . . . H30A H 0.7297 0.0249 0.6846 0.088 Uiso 1 1 calc R A . H30B H 0.6853 0.0357 0.7486 0.088 Uiso 1 1 calc R . . C31 C 0.7494(4) -0.0287(2) 0.7532(4) 0.096(2) Uani 1 1 d . A . H31A H 0.7982 -0.0395 0.7360 0.115 Uiso 1 1 calc R . . H31B H 0.7536 -0.0288 0.7996 0.115 Uiso 1 1 calc R . . C32 C 0.6946(6) -0.0625(4) 0.7353(5) 0.098(3) Uiso 0.70 1 d P . . H32A H 0.6466 -0.0532 0.7542 0.146 Uiso 0.70 1 calc PR A . H32B H 0.7088 -0.0955 0.7495 0.146 Uiso 0.70 1 calc PR . . H32C H 0.6897 -0.0624 0.6894 0.146 Uiso 0.70 1 calc PR . . C33 C 0.7152(3) 0.13362(19) 0.7534(2) 0.0520(12) Uani 1 1 d D A 1 H33A H 0.7131 0.1682 0.7384 0.062 Uiso 1 1 calc R A 1 H33B H 0.6743 0.1153 0.7324 0.062 Uiso 1 1 calc R A 1 C34 C 0.7011(3) 0.1333(2) 0.8233(3) 0.0718(16) Uani 1 1 d D A 1 H34A H 0.7440 0.1489 0.8451 0.086 Uiso 1 1 calc R A 1 H34B H 0.6977 0.0987 0.8380 0.086 Uiso 1 1 calc R A 1 C35' C 0.6173(15) 0.1333(9) 0.8288(12) 0.086(7) Uiso 0.30 1 d PD B 2 C35 C 0.6296(5) 0.1603(4) 0.8410(5) 0.085(3) Uiso 0.70 1 d PD A 1 H35A H 0.6326 0.1945 0.8245 0.102 Uiso 1 1 calc R A 1 H35B H 0.6269 0.1625 0.8874 0.102 Uiso 1 1 calc R A 1 C36 C 0.5558(9) 0.1362(6) 0.8163(8) 0.130(6) Uiso 0.55 1 d PD A 1 H36A H 0.5432 0.1502 0.7752 0.195 Uiso 1 1 calc R A 1 H36B H 0.5151 0.1429 0.8459 0.195 Uiso 1 1 calc R A 1 H36C H 0.5629 0.1005 0.8124 0.195 Uiso 1 1 calc R A 1 C36' C 0.5919(13) 0.1841(8) 0.8045(11) 0.138(8) Uiso 0.45 1 d PD B 2 C37 C 0.8692(3) 0.28298(15) 0.1392(2) 0.0471(11) Uani 1 1 d . . . H37A H 0.9094 0.3036 0.1576 0.056 Uiso 1 1 calc R . . H37B H 0.8375 0.3048 0.1130 0.056 Uiso 1 1 calc R . . C38 C 0.8217(3) 0.26300(18) 0.1922(3) 0.0613(14) Uani 1 1 d . . . H38A H 0.8536 0.2441 0.2217 0.074 Uiso 1 1 calc R . . H38B H 0.7832 0.2404 0.1751 0.074 Uiso 1 1 calc R . . C39 C 0.7840(4) 0.3052(2) 0.2267(3) 0.0784(18) Uani 1 1 d . . . H39A H 0.8229 0.3265 0.2457 0.094 Uiso 1 1 calc R . . H39B H 0.7555 0.3254 0.1962 0.094 Uiso 1 1 calc R . . C40 C 0.7312(4) 0.2877(3) 0.2779(4) 0.105(2) Uiso 1 1 d . . . H40A H 0.6962 0.2634 0.2604 0.158 Uiso 1 1 calc R . . H40B H 0.7030 0.3159 0.2944 0.158 Uiso 1 1 calc R . . H40C H 0.7602 0.2726 0.3119 0.158 Uiso 1 1 calc R . . C41 C 0.8459(3) 0.21401(17) 0.0637(3) 0.0604(15) Uani 1 1 d . . . H41A H 0.8154 0.1971 0.0960 0.072 Uiso 1 1 calc R C 1 H41B H 0.8713 0.1882 0.0386 0.072 Uiso 1 1 calc R C 1 C42 C 0.7938(4) 0.2430(2) 0.0208(4) 0.114(3) Uani 1 1 d . D 1 H42A H 0.7632 0.2656 0.0467 0.137 Uiso 1 1 calc R D 1 H42B H 0.8245 0.2635 -0.0078 0.137 Uiso 1 1 calc R D 1 C43 C 0.7419(4) 0.2109(3) -0.0184(4) 0.094(2) Uiso 1 1 d . D 1 H43A H 0.7130 0.2313 -0.0485 0.113 Uiso 1 1 calc R D 1 H43B H 0.7707 0.1859 -0.0421 0.113 Uiso 1 1 calc R D 1 C44' C 0.6496(17) 0.2170(12) -0.0099(14) 0.069(8) Uiso 0.20 1 d P E 2 C44 C 0.6971(4) 0.1897(3) 0.0223(4) 0.076(2) Uiso 0.80 1 d P D 1 H44A H 0.7244 0.1637 0.0448 0.114 Uiso 1 1 calc R D 1 H44B H 0.6543 0.1751 0.0001 0.114 Uiso 1 1 calc R D 1 H44C H 0.6791 0.2143 0.0524 0.114 Uiso 1 1 calc R D 1 C45 C 0.9515(3) 0.27341(15) 0.0492(2) 0.0476(12) Uani 1 1 d . . . H45A H 0.9181 0.2970 0.0274 0.057 Uiso 1 1 calc R D . H45B H 0.9893 0.2930 0.0724 0.057 Uiso 1 1 calc R . . C46 C 0.9919(3) 0.24301(17) 0.0000(2) 0.0514(12) Uani 1 1 d . D . H46A H 0.9551 0.2233 -0.0241 0.062 Uiso 1 1 calc R . . H46B H 1.0271 0.2200 0.0208 0.062 Uiso 1 1 calc R . . C47 C 1.0347(3) 0.27657(19) -0.0443(2) 0.0594(14) Uani 1 1 d . . . H47A H 0.9984 0.2966 -0.0686 0.071 Uiso 1 1 calc R D . H47B H 1.0658 0.2995 -0.0192 0.071 Uiso 1 1 calc R . . C48 C 1.0845(3) 0.2490(2) -0.0896(3) 0.0678(15) Uani 1 1 d . D . H48A H 1.1238 0.2317 -0.0662 0.102 Uiso 1 1 calc R . . H48B H 1.1075 0.2725 -0.1189 0.102 Uiso 1 1 calc R . . H48C H 1.0546 0.2250 -0.1132 0.102 Uiso 1 1 calc R . . C49 C 0.9541(3) 0.20938(15) 0.1331(2) 0.0445(11) Uani 1 1 d . . . H49A H 0.9223 0.1919 0.1640 0.053 Uiso 1 1 calc R D . H49B H 0.9738 0.1844 0.1035 0.053 Uiso 1 1 calc R . . C50 C 1.0192(3) 0.23213(18) 0.1678(2) 0.0532(12) Uani 1 1 d . D . H50A H 1.0011 0.2597 0.1942 0.064 Uiso 1 1 calc R . . H50B H 1.0554 0.2457 0.1371 0.064 Uiso 1 1 calc R . . C51 C 1.0580(3) 0.1941(2) 0.2089(2) 0.0600(14) Uani 1 1 d . . . H51A H 1.1073 0.2073 0.2222 0.072 Uiso 1 1 calc R D . H51B H 1.0672 0.1640 0.1838 0.072 Uiso 1 1 calc R . . C52 C 1.0135(4) 0.1803(2) 0.2671(3) 0.0788(18) Uani 1 1 d . D . H52A H 1.0040 0.2099 0.2922 0.118 Uiso 1 1 calc R . . H52B H 1.0421 0.1565 0.2922 0.118 Uiso 1 1 calc R . . H52C H 0.9657 0.1655 0.2545 0.118 Uiso 1 1 calc R . . C53 C 0.2051(2) -0.05139(16) 0.65804(19) 0.0363(9) Uani 1 1 d . F . H53A H 0.1877 -0.0589 0.6149 0.044 Uiso 1 1 calc R . . H53B H 0.2591 -0.0435 0.6556 0.044 Uiso 1 1 calc R . . C54 C 0.1958(3) -0.09749(18) 0.6979(2) 0.0513(12) Uani 1 1 d . . . H54A H 0.1418 -0.1040 0.7045 0.062 Uiso 1 1 calc R F . H54B H 0.2193 -0.0922 0.7395 0.062 Uiso 1 1 calc R . . C55 C 0.2318(3) -0.14216(19) 0.6661(3) 0.0591(13) Uani 1 1 d . F . H55A H 0.2849 -0.1342 0.6573 0.071 Uiso 1 1 calc R . . H55B H 0.2312 -0.1701 0.6960 0.071 Uiso 1 1 calc R . . C56 C 0.1960(5) -0.1582(2) 0.6071(3) 0.096(2) Uani 1 1 d . . . H56A H 0.1423 -0.1632 0.6141 0.143 Uiso 1 1 calc R F . H56B H 0.2187 -0.1892 0.5931 0.143 Uiso 1 1 calc R . . H56C H 0.2032 -0.1328 0.5748 0.143 Uiso 1 1 calc R . . C57 C 0.1920(2) 0.01018(17) 0.74528(18) 0.0394(10) Uani 1 1 d . F 1 H57A H 0.1622 0.0389 0.7593 0.047 Uiso 1 1 calc R F 1 H57B H 0.1826 -0.0170 0.7753 0.047 Uiso 1 1 calc R F 1 C58 C 0.2739(2) 0.02382(19) 0.7491(2) 0.0455(11) Uani 1 1 d D F 1 H58A H 0.2853 0.0493 0.7172 0.055 Uiso 1 1 calc R F 1 H58B H 0.3049 -0.0056 0.7399 0.055 Uiso 1 1 calc R F 1 C59 C 0.2935(3) 0.0433(2) 0.8139(3) 0.0655(15) Uani 1 1 d D F 1 H59A H 0.2816 0.0182 0.8461 0.079 Uiso 1 1 calc R F 1 H59B H 0.2639 0.0734 0.8229 0.079 Uiso 1 1 calc R F 1 C60 C 0.3815(4) 0.0561(3) 0.8159(4) 0.071(2) Uiso 0.80 1 d PD F 1 H60A H 0.4105 0.0258 0.8095 0.107 Uiso 1 1 calc R F 1 H60B H 0.3942 0.0704 0.8567 0.107 Uiso 1 1 calc R F 1 H60C H 0.3933 0.0798 0.7825 0.107 Uiso 1 1 calc R F 1 C60' C 0.2424(11) 0.0877(7) 0.8364(9) 0.031(4) Uiso 0.20 1 d P G 2 C61 C 0.1772(2) 0.03475(15) 0.63267(18) 0.0343(9) Uani 1 1 d . F 1 H61A H 0.2318 0.0405 0.6300 0.041 Uiso 1 1 calc R F 1 H61B H 0.1604 0.0224 0.5912 0.041 Uiso 1 1 calc R F 1 C62 C 0.1392(3) 0.08402(17) 0.6445(2) 0.0467(11) Uani 1 1 d . F 1 H62A H 0.0845 0.0791 0.6488 0.056 Uiso 1 1 calc R F 1 H62B H 0.1583 0.0987 0.6839 0.056 Uiso 1 1 calc R F 1 C63 C 0.1550(3) 0.11850(19) 0.5899(3) 0.0568(13) Uani 1 1 d . F 1 H63A H 0.2097 0.1239 0.5869 0.068 Uiso 1 1 calc R F 1 H63B H 0.1384 0.1025 0.5504 0.068 Uiso 1 1 calc R F 1 C64 C 0.1164(4) 0.1679(2) 0.5958(3) 0.084(2) Uani 1 1 d . F 1 H64A H 0.0620 0.1629 0.5970 0.125 Uiso 1 1 calc R F 1 H64B H 0.1293 0.1886 0.5597 0.125 Uiso 1 1 calc R F 1 H64C H 0.1327 0.1841 0.6346 0.125 Uiso 1 1 calc R F 1 C65 C 0.0806(2) -0.01580(17) 0.68838(19) 0.0379(10) Uani 1 1 d . F 1 H65A H 0.0738 -0.0412 0.7213 0.046 Uiso 1 1 calc R F 1 H65B H 0.0557 0.0147 0.7030 0.046 Uiso 1 1 calc R F 1 C66 C 0.0420(2) -0.0332(2) 0.6289(2) 0.0541(13) Uani 1 1 d . F 1 H66A H 0.0621 -0.0659 0.6169 0.065 Uiso 1 1 calc R F 1 H66B H 0.0530 -0.0099 0.5944 0.065 Uiso 1 1 calc R F 1 C67 C -0.0421(3) -0.0370(2) 0.6375(3) 0.0565(13) Uani 1 1 d . F 1 H67A H -0.0535 -0.0627 0.6692 0.068 Uiso 1 1 calc R F 1 H67B H -0.0618 -0.0052 0.6531 0.068 Uiso 1 1 calc R F 1 C68 C -0.0799(3) -0.0500(3) 0.5764(3) 0.089(2) Uani 1 1 d . F 1 H68A H -0.0638 -0.0269 0.5437 0.134 Uiso 1 1 calc R F 1 H68B H -0.1344 -0.0478 0.5816 0.134 Uiso 1 1 calc R F 1 H68C H -0.0662 -0.0836 0.5643 0.134 Uiso 1 1 calc R F 1 C69 C 0.5442(6) 0.8405(4) 0.0459(5) 0.059(3) Uiso 0.50 1 d P H 1 H69 H 0.5776 0.8659 0.0585 0.071 Uiso 0.50 1 calc PR H 1 C70 C 0.6090(9) 0.7925(7) 0.1163(8) 0.116(5) Uiso 0.50 1 d P H 1 H70A H 0.6384 0.8228 0.1206 0.173 Uiso 0.50 1 calc PR H 1 H70B H 0.6417 0.7655 0.1028 0.173 Uiso 0.50 1 calc PR H 1 H70C H 0.5862 0.7841 0.1567 0.173 Uiso 0.50 1 calc PR H 1 C71 C 0.5064(8) 0.7578(5) 0.0570(7) 0.094(4) Uiso 0.50 1 d P H 1 H71A H 0.4708 0.7522 0.0912 0.141 Uiso 0.50 1 calc PR H 1 H71B H 0.5378 0.7285 0.0516 0.141 Uiso 0.50 1 calc PR H 1 H71C H 0.4789 0.7643 0.0180 0.141 Uiso 0.50 1 calc PR H 1 C72 C 0.8234(3) 0.3373(2) 0.8792(3) 0.0674(15) Uiso 1 1 d . I 1 H72 H 0.8344 0.3503 0.9196 0.081 Uiso 1 1 calc R I 1 C73 C 0.7329(6) 0.3045(4) 0.8109(5) 0.153(4) Uiso 1 1 d . I 1 H73A H 0.7746 0.3043 0.7810 0.229 Uiso 1 1 calc R I 1 H73B H 0.6908 0.3229 0.7930 0.229 Uiso 1 1 calc R I 1 H73C H 0.7173 0.2705 0.8196 0.229 Uiso 1 1 calc R I 1 C74 C 0.6974(4) 0.3393(3) 0.9105(3) 0.088(2) Uiso 1 1 d . I 1 H74A H 0.7190 0.3531 0.9491 0.132 Uiso 1 1 calc R I 1 H74B H 0.6690 0.3095 0.9207 0.132 Uiso 1 1 calc R I 1 H74C H 0.6639 0.3637 0.8913 0.132 Uiso 1 1 calc R I 1 C75 C 0.3565(4) 0.0254(3) 0.9811(4) 0.089(2) Uiso 1 1 d . J 1 H75 H 0.3619 0.0124 0.9399 0.107 Uiso 1 1 calc R J 1 C76 C 0.3945(4) -0.0550(3) 1.0182(4) 0.104(2) Uiso 1 1 d . J 1 H76A H 0.3560 -0.0757 1.0377 0.156 Uiso 1 1 calc R J 1 H76B H 0.4429 -0.0613 1.0385 0.156 Uiso 1 1 calc R J 1 H76C H 0.3980 -0.0628 0.9734 0.156 Uiso 1 1 calc R J 1 C77 C 0.3464(6) 0.0086(4) 1.0892(5) 0.136(3) Uiso 1 1 d . J 1 H77A H 0.3258 0.0422 1.0889 0.204 Uiso 1 1 calc R J 1 H77B H 0.3875 0.0067 1.1196 0.204 Uiso 1 1 calc R J 1 H77C H 0.3070 -0.0148 1.1010 0.204 Uiso 1 1 calc R J 1 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 0.02822(17) 0.02195(16) 0.02462(16) 0.00062(13) -0.00113(13) 0.00656(13) Mo2 0.02919(17) 0.02030(15) 0.02236(15) -0.00176(12) 0.00517(13) 0.00408(13) Mo3 0.03122(18) 0.02833(17) 0.01822(15) 0.00191(13) 0.00034(13) 0.00520(14) Mo4 0.02518(17) 0.02560(17) 0.03568(18) 0.00695(14) -0.00310(14) 0.00601(13) Mo5 0.02217(16) 0.02226(16) 0.03276(17) 0.00245(13) 0.00517(13) 0.00104(12) Mo6 0.01589(15) 0.03015(17) 0.03295(18) 0.00033(14) -0.00004(13) 0.00362(13) Mn1 0.0223(4) 0.0175(3) 0.0172(3) -0.0009(3) 0.0004(3) 0.0023(3) Mn2 0.0148(3) 0.0199(4) 0.0250(4) 0.0019(3) 0.0006(3) 0.0027(3) O1 0.0311(14) 0.0239(13) 0.0214(12) 0.0001(10) 0.0048(10) 0.0022(11) O2 0.0339(15) 0.0313(15) 0.0380(15) 0.0013(12) 0.0100(12) 0.0079(12) O3 0.0496(17) 0.0265(14) 0.0270(14) -0.0047(11) 0.0038(12) 0.0018(12) O4 0.0309(14) 0.0179(12) 0.0257(13) -0.0017(10) 0.0020(11) 0.0029(10) O5 0.0319(15) 0.0343(15) 0.0407(16) -0.0015(13) -0.0022(12) 0.0090(12) O6 0.0249(13) 0.0166(11) 0.0231(12) -0.0011(10) 0.0009(10) 0.0013(10) O7 0.0264(13) 0.0204(12) 0.0229(12) -0.0013(10) 0.0017(10) -0.0005(10) O8 0.0240(13) 0.0212(12) 0.0229(12) 0.0007(10) 0.0006(10) 0.0019(10) O9 0.0477(17) 0.0257(14) 0.0339(15) 0.0037(12) -0.0032(13) 0.0052(12) O10 0.0300(14) 0.0282(13) 0.0242(13) -0.0007(11) -0.0056(11) 0.0057(11) O11 0.0459(18) 0.0406(16) 0.0362(16) 0.0136(13) 0.0042(13) 0.0056(14) O12 0.0410(17) 0.0540(18) 0.0257(14) -0.0093(13) -0.0018(12) 0.0035(14) O13 0.0193(12) 0.0266(13) 0.0332(14) 0.0013(11) 0.0073(10) 0.0025(10) O14 0.0406(16) 0.0327(15) 0.0361(15) 0.0035(12) 0.0072(13) 0.0028(13) O15 0.0274(14) 0.0294(14) 0.0452(16) -0.0018(12) 0.0064(12) -0.0008(11) O16 0.0434(17) 0.0474(18) 0.0385(16) 0.0127(14) -0.0030(13) 0.0023(14) O17 0.0257(13) 0.0197(12) 0.0383(14) 0.0027(11) 0.0025(11) 0.0029(10) O18 0.0188(12) 0.0246(12) 0.0277(13) -0.0022(10) 0.0027(10) 0.0017(10) O19 0.0215(13) 0.0239(13) 0.0297(13) -0.0016(11) -0.0003(10) 0.0017(10) O20 0.0200(13) 0.0357(15) 0.0305(14) 0.0015(11) -0.0031(11) 0.0056(11) O21 0.0253(13) 0.0241(13) 0.0296(13) -0.0009(11) 0.0016(11) 0.0001(10) O22 0.0269(15) 0.0484(18) 0.0439(16) -0.0053(14) -0.0002(12) -0.0075(13) O23 0.0278(15) 0.0464(17) 0.0474(17) 0.0009(14) 0.0031(13) 0.0155(13) O24 0.0322(15) 0.0327(15) 0.0611(19) 0.0043(14) -0.0033(14) 0.0103(12) O25 0.0314(15) 0.0288(15) 0.0577(19) -0.0124(13) 0.0067(14) -0.0015(12) O26 0.0455(18) 0.0358(16) 0.058(2) -0.0028(15) -0.0014(15) 0.0103(14) O27 0.056(2) 0.050(2) 0.050(2) -0.0146(16) -0.0001(16) -0.0052(16) O28 0.0347(16) 0.0464(17) 0.0415(16) -0.0173(14) 0.0140(13) -0.0122(14) O29 0.0397(18) 0.056(2) 0.0516(19) -0.0012(16) 0.0033(15) -0.0096(15) O30 0.0455(19) 0.054(2) 0.055(2) -0.0034(16) 0.0020(16) -0.0031(16) O32 0.057(2) 0.067(3) 0.133(4) -0.036(3) 0.023(2) -0.019(2) O33 0.051(2) 0.056(2) 0.107(3) 0.005(2) 0.020(2) 0.0153(18) N1 0.0223(16) 0.0241(16) 0.0376(18) -0.0047(14) 0.0011(13) -0.0001(13) N2 0.0233(16) 0.0324(17) 0.0380(18) -0.0128(15) 0.0009(14) -0.0062(13) N3 0.059(2) 0.039(2) 0.041(2) 0.0097(17) -0.0230(19) 0.0015(18) N4 0.051(2) 0.0211(17) 0.069(3) -0.0052(17) -0.009(2) 0.0068(16) N5 0.0250(17) 0.044(2) 0.0266(16) 0.0029(15) 0.0048(13) 0.0019(14) N7 0.052(3) 0.069(3) 0.067(3) -0.019(2) -0.016(2) -0.009(2) N8 0.111(4) 0.056(3) 0.054(3) -0.001(2) -0.007(3) 0.022(3) C1 0.0254(19) 0.0202(17) 0.0296(19) 0.0007(15) -0.0008(15) -0.0007(14) C2 0.0246(19) 0.0233(18) 0.033(2) -0.0046(16) -0.0001(15) -0.0014(15) C3 0.030(2) 0.0239(18) 0.0284(19) -0.0036(15) -0.0010(16) -0.0040(15) C4 0.0285(19) 0.0182(17) 0.0300(19) 0.0005(15) 0.0027(15) -0.0016(15) C5 0.031(2) 0.0257(19) 0.041(2) -0.0057(17) 0.0004(18) -0.0027(17) C6 0.031(2) 0.028(2) 0.060(3) -0.009(2) 0.004(2) -0.0016(17) C7 0.033(2) 0.032(2) 0.064(3) -0.008(2) -0.011(2) 0.0001(18) C8 0.029(2) 0.028(2) 0.061(3) -0.004(2) -0.014(2) -0.0035(17) C9 0.067(4) 0.049(3) 0.079(4) 0.000(3) -0.031(3) 0.013(3) C10 0.034(3) 0.046(3) 0.104(4) -0.023(3) -0.009(3) 0.003(2) C11 0.0233(19) 0.0267(19) 0.0297(19) -0.0063(16) 0.0040(15) -0.0006(15) C12 0.0260(19) 0.031(2) 0.031(2) -0.0053(16) 0.0003(16) 0.0015(16) C13 0.0254(19) 0.029(2) 0.033(2) -0.0061(16) 0.0055(16) -0.0005(16) C14 0.0266(19) 0.0252(19) 0.032(2) -0.0058(16) 0.0030(16) 0.0015(15) C15 0.029(2) 0.039(2) 0.040(2) -0.0110(19) 0.0062(18) -0.0039(18) C16 0.042(3) 0.049(3) 0.049(3) -0.017(2) 0.013(2) -0.018(2) C17 0.036(2) 0.065(3) 0.045(3) -0.019(2) 0.003(2) -0.015(2) C18 0.044(3) 0.048(3) 0.030(2) -0.010(2) 0.0029(19) -0.010(2) C19 0.066(4) 0.099(5) 0.058(3) -0.040(3) 0.018(3) -0.044(3) C20 0.045(3) 0.097(5) 0.059(3) -0.003(3) -0.003(3) -0.011(3) C21 0.053(3) 0.047(3) 0.045(3) 0.003(2) -0.026(2) 0.001(2) C22 0.066(4) 0.046(3) 0.099(5) 0.010(3) -0.028(3) 0.001(3) C23 0.066(4) 0.052(3) 0.067(3) 0.004(3) -0.010(3) -0.012(3) C24 0.082(4) 0.060(4) 0.098(5) 0.023(3) 0.006(4) -0.009(3) C25 0.061(3) 0.049(3) 0.042(3) 0.002(2) -0.016(2) 0.007(2) C26 0.090(5) 0.081(4) 0.062(4) -0.003(3) -0.014(3) 0.025(4) C27 0.070(4) 0.055(3) 0.066(3) -0.017(3) -0.009(3) 0.005(3) C29 0.082(4) 0.044(3) 0.056(3) 0.011(2) -0.036(3) -0.001(3) C30 0.102(5) 0.047(3) 0.072(4) 0.016(3) -0.043(4) -0.013(3) C31 0.122(6) 0.050(4) 0.115(6) 0.012(4) -0.053(5) -0.021(4) C33 0.055(3) 0.052(3) 0.048(3) 0.010(2) -0.013(2) -0.001(2) C34 0.080(4) 0.080(4) 0.055(3) 0.010(3) -0.006(3) -0.002(3) C37 0.054(3) 0.024(2) 0.064(3) -0.002(2) 0.002(2) 0.005(2) C38 0.061(3) 0.040(3) 0.083(4) -0.001(3) 0.008(3) 0.001(2) C39 0.088(5) 0.062(4) 0.085(4) 0.009(3) 0.032(4) 0.018(3) C41 0.050(3) 0.033(2) 0.098(4) -0.018(3) -0.023(3) 0.009(2) C42 0.095(5) 0.059(4) 0.189(8) -0.040(5) -0.091(6) 0.027(4) C45 0.062(3) 0.023(2) 0.057(3) -0.002(2) -0.010(2) 0.009(2) C46 0.059(3) 0.033(2) 0.063(3) -0.014(2) -0.012(3) 0.009(2) C47 0.073(4) 0.046(3) 0.059(3) 0.000(3) -0.011(3) 0.007(3) C48 0.076(4) 0.073(4) 0.054(3) -0.009(3) -0.004(3) 0.008(3) C49 0.045(3) 0.026(2) 0.063(3) 0.002(2) -0.006(2) 0.0038(19) C50 0.049(3) 0.049(3) 0.062(3) 0.002(2) -0.003(2) -0.003(2) C51 0.057(3) 0.066(3) 0.057(3) -0.002(3) -0.008(3) 0.010(3) C52 0.100(5) 0.079(4) 0.058(4) 0.001(3) -0.011(3) 0.000(4) C53 0.029(2) 0.045(2) 0.035(2) -0.0007(19) 0.0050(17) 0.0030(18) C54 0.053(3) 0.052(3) 0.049(3) 0.015(2) 0.004(2) 0.007(2) C55 0.059(3) 0.047(3) 0.071(4) 0.008(3) -0.002(3) 0.001(2) C56 0.137(7) 0.057(4) 0.092(5) -0.009(4) -0.036(5) 0.002(4) C57 0.039(2) 0.053(3) 0.026(2) 0.0006(19) 0.0049(17) 0.003(2) C58 0.037(2) 0.057(3) 0.043(2) -0.003(2) -0.004(2) 0.002(2) C59 0.074(4) 0.059(3) 0.064(3) -0.011(3) -0.024(3) 0.007(3) C61 0.030(2) 0.047(2) 0.0262(19) 0.0055(18) 0.0078(16) 0.0021(18) C62 0.039(3) 0.049(3) 0.051(3) 0.005(2) 0.012(2) 0.004(2) C63 0.049(3) 0.051(3) 0.071(3) 0.016(3) 0.020(3) 0.007(2) C64 0.081(4) 0.062(4) 0.108(5) 0.022(4) 0.023(4) 0.012(3) C65 0.024(2) 0.055(3) 0.035(2) 0.004(2) 0.0075(17) -0.0025(19) C66 0.032(2) 0.080(4) 0.051(3) -0.002(3) 0.001(2) -0.006(2) C67 0.033(3) 0.067(3) 0.070(3) -0.002(3) -0.005(2) 0.000(2) C68 0.040(3) 0.128(6) 0.100(5) -0.014(5) -0.012(3) -0.015(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O5 1.703(3) . ? Mo1 O9 1.705(3) . ? Mo1 O10 1.921(2) . ? Mo1 O4 1.934(2) . ? Mo1 O8 2.309(2) . ? Mo1 O6 2.408(2) . ? Mo2 O3 1.698(3) . ? Mo2 O2 1.714(3) . ? Mo2 O4 1.912(2) . ? Mo2 O1 1.913(2) . ? Mo2 O7 2.356(2) . ? Mo2 O6 2.364(2) . ? Mo3 O12 1.703(3) . ? Mo3 O11 1.703(3) . ? Mo3 O1 1.924(2) 3_575 ? Mo3 O10 1.927(3) . ? Mo3 O8 2.326(2) . ? Mo3 O7 2.413(2) 3_575 ? Mo4 O16 1.700(3) . ? Mo4 O24 1.719(3) . ? Mo4 O17 1.907(3) . ? Mo4 O20 1.916(3) . ? Mo4 O21 2.358(2) . ? Mo4 O19 2.387(2) . ? Mo5 O14 1.700(3) . ? Mo5 O15 1.713(3) . ? Mo5 O13 1.912(2) . ? Mo5 O17 1.932(2) . ? Mo5 O19 2.326(2) . ? Mo5 O18 2.381(2) . ? Mo6 O23 1.703(3) . ? Mo6 O22 1.704(3) . ? Mo6 O20 1.926(3) . ? Mo6 O13 1.933(2) 3_767 ? Mo6 O21 2.312(2) . ? Mo6 O18 2.403(2) 3_767 ? Mn1 O6 1.919(2) . ? Mn1 O6 1.919(2) 3_575 ? Mn1 O7 1.939(2) . ? Mn1 O7 1.939(2) 3_575 ? Mn1 O8 2.103(2) . ? Mn1 O8 2.103(2) 3_575 ? Mn2 O18 1.895(2) 3_767 ? Mn2 O18 1.895(2) . ? Mn2 O19 2.005(2) 3_767 ? Mn2 O19 2.005(2) . ? Mn2 O21 2.057(2) 3_767 ? Mn2 O21 2.057(2) . ? O1 Mo3 1.924(2) 3_575 ? O6 C2 1.436(4) . ? O7 C3 1.449(4) . ? O7 Mo3 2.413(2) 3_575 ? O8 C4 1.434(4) . ? O13 Mo6 1.933(2) 3_767 ? O18 C13 1.432(4) . ? O18 Mo6 2.403(2) 3_767 ? O19 C12 1.443(4) . ? O21 C14 1.436(4) . ? O25 C5 1.223(5) . ? O26 C8 1.336(5) . ? O27 C8 1.205(5) . ? O28 C15 1.233(5) . ? O29 C18 1.322(5) . ? O30 C18 1.209(5) . ? O31 C69 1.232(13) . ? O32 C72 1.278(7) . ? O33 C75 1.223(8) . ? N1 C5 1.351(5) . ? N1 C1 1.469(5) . ? N2 C15 1.338(5) . ? N2 C11 1.476(5) . ? N3 C25 1.509(6) . ? N3 C33 1.521(6) . ? N3 C21 1.524(6) . ? N3 C29 1.526(6) . ? N4 C49 1.513(5) . ? N4 C37 1.516(6) . ? N4 C45 1.517(6) . ? N4 C41 1.521(6) . ? N5 C65 1.516(5) . ? N5 C57 1.519(5) . ? N5 C61 1.523(5) . ? N5 C53 1.526(5) . ? N6 C69 1.247(13) . ? N6 C70 1.387(17) . ? N6 C71 1.441(16) . ? N7 C72 1.254(7) . ? N7 C73 1.416(10) . ? N7 C74 1.433(8) . ? N8 C75 1.277(8) . ? N8 C76 1.441(8) . ? N8 C77 1.483(10) . ? C1 C3 1.538(5) 3_575 ? C1 C2 1.544(5) . ? C1 C4 1.545(5) 3_575 ? C3 C1 1.538(5) 3_575 ? C4 C1 1.545(5) 3_575 ? C5 C6 1.523(5) . ? C6 C7 1.534(6) . ? C7 C9 1.512(7) . ? C7 C8 1.527(6) . ? C7 C10 1.539(6) . ? C11 C14 1.537(5) 3_767 ? C11 C13 1.541(5) 3_767 ? C11 C12 1.546(5) . ? C13 C11 1.541(5) 3_767 ? C14 C11 1.537(5) 3_767 ? C15 C16 1.525(6) . ? C16 C17 1.518(6) . ? C17 C18 1.528(6) . ? C17 C20 1.530(8) . ? C17 C19 1.547(7) . ? C21 C22 1.517(7) . ? C22 C23 1.521(7) . ? C23 C24 1.486(8) . ? C25 C26 1.505(8) . ? C26 C27 1.531(8) . ? C27 C28 1.462(9) . ? C29 C30 1.512(7) . ? C30 C31 1.534(8) . ? C31 C32 1.393(11) . ? C33 C34 1.510(7) . ? C34 C35 1.521(10) . ? C35' C36' 1.539(18) . ? C35 C36 1.561(13) . ? C37 C38 1.513(7) . ? C38 C39 1.518(7) . ? C39 C40 1.517(9) . ? C41 C42 1.522(8) . ? C42 C43 1.519(9) . ? C43 C44 1.314(9) . ? C45 C46 1.517(6) . ? C46 C47 1.518(7) . ? C47 C48 1.511(7) . ? C49 C50 1.508(6) . ? C50 C51 1.520(7) . ? C51 C52 1.520(8) . ? C53 C54 1.519(6) . ? C54 C55 1.530(7) . ? C55 C56 1.474(8) . ? C57 C58 1.511(6) . ? C58 C59 1.517(6) . ? C59 C60 1.608(8) . ? C61 C62 1.519(6) . ? C62 C63 1.518(6) . ? C63 C64 1.510(7) . ? C65 C66 1.515(6) . ? C66 C67 1.517(6) . ? C67 C68 1.505(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mo1 O9 105.31(13) . . ? O5 Mo1 O10 97.36(12) . . ? O9 Mo1 O10 103.22(12) . . ? O5 Mo1 O4 101.18(12) . . ? O9 Mo1 O4 99.47(11) . . ? O10 Mo1 O4 145.61(10) . . ? O5 Mo1 O8 158.36(11) . . ? O9 Mo1 O8 95.40(11) . . ? O10 Mo1 O8 71.36(9) . . ? O4 Mo1 O8 81.14(9) . . ? O5 Mo1 O6 88.35(11) . . ? O9 Mo1 O6 164.65(11) . . ? O10 Mo1 O6 81.46(9) . . ? O4 Mo1 O6 70.47(9) . . ? O8 Mo1 O6 72.01(8) . . ? O3 Mo2 O2 105.79(13) . . ? O3 Mo2 O4 100.48(11) . . ? O2 Mo2 O4 101.61(12) . . ? O3 Mo2 O1 101.06(11) . . ? O2 Mo2 O1 98.58(12) . . ? O4 Mo2 O1 145.06(10) . . ? O3 Mo2 O7 93.27(11) . . ? O2 Mo2 O7 160.16(11) . . ? O4 Mo2 O7 79.79(9) . . ? O1 Mo2 O7 71.82(9) . . ? O3 Mo2 O6 161.34(11) . . ? O2 Mo2 O6 92.55(11) . . ? O4 Mo2 O6 71.83(9) . . ? O1 Mo2 O6 79.09(9) . . ? O7 Mo2 O6 68.88(8) . . ? O12 Mo3 O11 104.89(14) . . ? O12 Mo3 O1 101.65(12) . 3_575 ? O11 Mo3 O1 99.00(12) . 3_575 ? O12 Mo3 O10 97.29(12) . . ? O11 Mo3 O10 104.07(12) . . ? O1 Mo3 O10 145.14(10) 3_575 . ? O12 Mo3 O8 158.82(12) . . ? O11 Mo3 O8 95.19(12) . . ? O1 Mo3 O8 81.41(9) 3_575 . ? O10 Mo3 O8 70.87(9) . . ? O12 Mo3 O7 88.60(12) . 3_575 ? O11 Mo3 O7 164.50(12) . 3_575 ? O1 Mo3 O7 70.32(9) 3_575 3_575 ? O10 Mo3 O7 81.26(9) . 3_575 ? O8 Mo3 O7 72.55(8) . 3_575 ? O16 Mo4 O24 105.70(14) . . ? O16 Mo4 O17 102.43(13) . . ? O24 Mo4 O17 99.36(12) . . ? O16 Mo4 O20 98.04(13) . . ? O24 Mo4 O20 102.56(12) . . ? O17 Mo4 O20 144.55(10) . . ? O16 Mo4 O21 160.59(12) . . ? O24 Mo4 O21 92.30(12) . . ? O17 Mo4 O21 81.24(10) . . ? O20 Mo4 O21 70.43(9) . . ? O16 Mo4 O19 90.41(12) . . ? O24 Mo4 O19 162.66(12) . . ? O17 Mo4 O19 70.31(9) . . ? O20 Mo4 O19 81.00(9) . . ? O21 Mo4 O19 72.72(8) . . ? O14 Mo5 O15 105.63(13) . . ? O14 Mo5 O13 100.09(12) . . ? O15 Mo5 O13 101.55(12) . . ? O14 Mo5 O17 102.84(12) . . ? O15 Mo5 O17 96.90(11) . . ? O13 Mo5 O17 145.33(10) . . ? O14 Mo5 O19 94.86(11) . . ? O15 Mo5 O19 158.37(11) . . ? O13 Mo5 O19 81.15(9) . . ? O17 Mo5 O19 71.35(9) . . ? O14 Mo5 O18 163.54(11) . . ? O15 Mo5 O18 90.23(11) . . ? O13 Mo5 O18 71.83(9) . . ? O17 Mo5 O18 79.06(9) . . ? O19 Mo5 O18 70.04(8) . . ? O23 Mo6 O22 106.18(14) . . ? O23 Mo6 O20 103.17(12) . . ? O22 Mo6 O20 97.85(13) . . ? O23 Mo6 O13 99.19(12) . 3_767 ? O22 Mo6 O13 101.00(13) . 3_767 ? O20 Mo6 O13 145.31(10) . 3_767 ? O23 Mo6 O21 96.31(12) . . ? O22 Mo6 O21 156.89(11) . . ? O20 Mo6 O21 71.33(10) . . ? O13 Mo6 O21 80.18(10) 3_767 . ? O23 Mo6 O18 164.35(12) . 3_767 ? O22 Mo6 O18 87.97(11) . 3_767 ? O20 Mo6 O18 80.93(9) . 3_767 ? O13 Mo6 O18 70.97(9) 3_767 3_767 ? O21 Mo6 O18 70.44(8) . 3_767 ? O6 Mn1 O6 180.0 . 3_575 ? O6 Mn1 O7 87.59(10) . . ? O6 Mn1 O7 92.41(10) 3_575 . ? O6 Mn1 O7 92.41(10) . 3_575 ? O6 Mn1 O7 87.59(10) 3_575 3_575 ? O7 Mn1 O7 180.00(14) . 3_575 ? O6 Mn1 O8 87.09(9) . . ? O6 Mn1 O8 92.91(9) 3_575 . ? O7 Mn1 O8 92.23(9) . . ? O7 Mn1 O8 87.77(9) 3_575 . ? O6 Mn1 O8 92.91(9) . 3_575 ? O6 Mn1 O8 87.09(9) 3_575 3_575 ? O7 Mn1 O8 87.77(9) . 3_575 ? O7 Mn1 O8 92.23(9) 3_575 3_575 ? O8 Mn1 O8 180.00(12) . 3_575 ? O18 Mn2 O18 180.00(11) 3_767 . ? O18 Mn2 O19 87.63(10) 3_767 3_767 ? O18 Mn2 O19 92.37(10) . 3_767 ? O18 Mn2 O19 92.37(10) 3_767 . ? O18 Mn2 O19 87.63(10) . . ? O19 Mn2 O19 180.000(1) 3_767 . ? O18 Mn2 O21 93.11(10) 3_767 3_767 ? O18 Mn2 O21 86.89(10) . 3_767 ? O19 Mn2 O21 87.67(10) 3_767 3_767 ? O19 Mn2 O21 92.33(10) . 3_767 ? O18 Mn2 O21 86.89(10) 3_767 . ? O18 Mn2 O21 93.11(10) . . ? O19 Mn2 O21 92.33(10) 3_767 . ? O19 Mn2 O21 87.67(10) . . ? O21 Mn2 O21 180.000(1) 3_767 . ? Mo2 O1 Mo3 121.98(13) . 3_575 ? Mo2 O4 Mo1 121.87(12) . . ? C2 O6 Mn1 117.3(2) . . ? C2 O6 Mo2 119.5(2) . . ? Mn1 O6 Mo2 101.93(10) . . ? C2 O6 Mo1 122.0(2) . . ? Mn1 O6 Mo1 101.54(10) . . ? Mo2 O6 Mo1 89.53(8) . . ? C3 O7 Mn1 117.7(2) . . ? C3 O7 Mo2 120.4(2) . . ? Mn1 O7 Mo2 101.60(10) . . ? C3 O7 Mo3 121.5(2) . 3_575 ? Mn1 O7 Mo3 100.80(9) . 3_575 ? Mo2 O7 Mo3 89.41(8) . 3_575 ? C4 O8 Mn1 113.84(19) . . ? C4 O8 Mo1 123.3(2) . . ? Mn1 O8 Mo1 99.35(9) . . ? C4 O8 Mo3 123.4(2) . . ? Mn1 O8 Mo3 98.85(9) . . ? Mo1 O8 Mo3 92.79(8) . . ? Mo1 O10 Mo3 121.42(13) . . ? Mo5 O13 Mo6 121.61(13) . 3_767 ? Mo4 O17 Mo5 121.89(13) . . ? C13 O18 Mn2 117.4(2) . . ? C13 O18 Mo5 119.2(2) . . ? Mn2 O18 Mo5 101.89(10) . . ? C13 O18 Mo6 121.9(2) . 3_767 ? Mn2 O18 Mo6 102.23(10) . 3_767 ? Mo5 O18 Mo6 89.12(8) . 3_767 ? C12 O19 Mn2 116.4(2) . . ? C12 O19 Mo5 121.9(2) . . ? Mn2 O19 Mo5 100.43(10) . . ? C12 O19 Mo4 122.0(2) . . ? Mn2 O19 Mo4 100.09(10) . . ? Mo5 O19 Mo4 90.79(8) . . ? Mo4 O20 Mo6 121.93(13) . . ? C14 O21 Mn2 114.8(2) . . ? C14 O21 Mo6 121.7(2) . . ? Mn2 O21 Mo6 100.43(10) . . ? C14 O21 Mo4 123.4(2) . . ? Mn2 O21 Mo4 99.50(10) . . ? Mo6 O21 Mo4 91.98(9) . . ? C5 N1 C1 126.7(3) . . ? C15 N2 C11 126.3(3) . . ? C25 N3 C33 105.6(3) . . ? C25 N3 C21 111.5(4) . . ? C33 N3 C21 111.1(4) . . ? C25 N3 C29 110.7(4) . . ? C33 N3 C29 112.1(4) . . ? C21 N3 C29 106.1(3) . . ? C49 N4 C37 111.8(4) . . ? C49 N4 C45 110.5(4) . . ? C37 N4 C45 106.5(3) . . ? C49 N4 C41 106.6(3) . . ? C37 N4 C41 110.8(4) . . ? C45 N4 C41 110.7(4) . . ? C65 N5 C57 106.5(3) . . ? C65 N5 C61 110.9(3) . . ? C57 N5 C61 110.7(3) . . ? C65 N5 C53 111.1(3) . . ? C57 N5 C53 110.9(3) . . ? C61 N5 C53 106.8(3) . . ? C69 N6 C70 121.1(12) . . ? C69 N6 C71 121.8(10) . . ? C70 N6 C71 117.1(12) . . ? C72 N7 C73 122.8(7) . . ? C72 N7 C74 121.8(5) . . ? C73 N7 C74 115.4(6) . . ? C75 N8 C76 125.2(6) . . ? C75 N8 C77 116.8(6) . . ? C76 N8 C77 113.8(6) . . ? N1 C1 C3 109.1(3) . 3_575 ? N1 C1 C2 103.2(3) . . ? C3 C1 C2 110.8(3) 3_575 . ? N1 C1 C4 107.3(3) . 3_575 ? C3 C1 C4 113.3(3) 3_575 3_575 ? C2 C1 C4 112.5(3) . 3_575 ? O6 C2 C1 114.2(3) . . ? O7 C3 C1 112.8(3) . 3_575 ? O8 C4 C1 114.2(3) . 3_575 ? O25 C5 N1 124.5(4) . . ? O25 C5 C6 121.3(3) . . ? N1 C5 C6 114.2(3) . . ? C5 C6 C7 113.3(4) . . ? C9 C7 C8 110.2(4) . . ? C9 C7 C6 110.7(4) . . ? C8 C7 C6 111.4(3) . . ? C9 C7 C10 110.4(4) . . ? C8 C7 C10 106.2(3) . . ? C6 C7 C10 107.8(4) . . ? O27 C8 O26 123.2(4) . . ? O27 C8 C7 124.6(4) . . ? O26 C8 C7 112.0(4) . . ? N2 C11 C14 107.4(3) . 3_767 ? N2 C11 C13 102.1(3) . 3_767 ? C14 C11 C13 112.0(3) 3_767 3_767 ? N2 C11 C12 109.2(3) . . ? C14 C11 C12 114.1(3) 3_767 . ? C13 C11 C12 111.1(3) 3_767 . ? O19 C12 C11 112.6(3) . . ? O18 C13 C11 114.3(3) . 3_767 ? O21 C14 C11 113.6(3) . 3_767 ? O28 C15 N2 123.9(4) . . ? O28 C15 C16 121.4(4) . . ? N2 C15 C16 114.7(3) . . ? C17 C16 C15 112.3(4) . . ? C16 C17 C18 109.0(4) . . ? C16 C17 C20 110.6(4) . . ? C18 C17 C20 113.1(4) . . ? C16 C17 C19 107.5(4) . . ? C18 C17 C19 106.1(4) . . ? C20 C17 C19 110.2(4) . . ? O30 C18 O29 123.5(4) . . ? O30 C18 C17 122.2(4) . . ? O29 C18 C17 114.1(4) . . ? C22 C21 N3 115.9(4) . . ? C21 C22 C23 111.4(4) . . ? C24 C23 C22 113.1(5) . . ? C26 C25 N3 116.5(4) . . ? C25 C26 C27 110.8(5) . . ? C28 C27 C26 113.7(5) . . ? C30 C29 N3 115.4(4) . . ? C29 C30 C31 108.8(5) . . ? C32 C31 C30 113.4(7) . . ? C34 C33 N3 114.9(4) . . ? C33 C34 C35 112.5(6) . . ? C34 C35 C36 115.0(10) . . ? C38 C37 N4 116.2(4) . . ? C37 C38 C39 110.0(4) . . ? C40 C39 C38 112.9(5) . . ? N4 C41 C42 114.6(4) . . ? C43 C42 C41 114.0(5) . . ? C44 C43 C42 105.1(7) . . ? C46 C45 N4 116.4(4) . . ? C45 C46 C47 110.2(4) . . ? C48 C47 C46 113.5(4) . . ? C50 C49 N4 115.7(4) . . ? C49 C50 C51 110.8(4) . . ? C50 C51 C52 113.5(5) . . ? C54 C53 N5 115.8(3) . . ? C53 C54 C55 110.9(4) . . ? C56 C55 C54 115.3(5) . . ? C58 C57 N5 116.1(3) . . ? C57 C58 C59 110.9(4) . . ? C58 C59 C60 108.8(5) . . ? C62 C61 N5 116.6(3) . . ? C63 C62 C61 109.3(4) . . ? C64 C63 C62 113.3(4) . . ? C66 C65 N5 114.4(3) . . ? C65 C66 C67 111.7(4) . . ? C68 C67 C66 110.8(5) . . ? O31 C69 N6 127.7(12) . . ? N7 C72 O32 125.9(6) . . ? O33 C75 N8 129.1(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.33 _refine_diff_density_min -0.66 _refine_diff_density_rms 0.09 data_mh242cy _database_code_depnum_ccdc_archive 'CCDC 909168' #TrackingRef 'MnMo6-6-MeCN.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H146 Mn Mo6 N7 O30' _chemical_formula_weight 2220.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.2400(6) _cell_length_b 27.2040(11) _cell_length_c 20.4735(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.794(2) _cell_angle_gamma 90.00 _cell_volume 9597.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6262 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 22.2 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4576 _exptl_absorpt_coefficient_mu 0.961 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8615 _exptl_absorpt_correction_T_max 0.9626 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Quasar CCD' _diffrn_measurement_method '\w & \p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 74010 _diffrn_reflns_av_R_equivalents 0.1093 _diffrn_reflns_av_sigmaI/netI 0.1206 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.00 _reflns_number_total 18657 _reflns_number_gt 10601 _reflns_threshold_expression >2\s(I) _computing_data_collection Apex2 _computing_cell_refinement Apex2 _computing_data_reduction Apex2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Diamond3 _computing_publication_material WinGX _refine_special_details ; DFIX restraints were applied a number of C-C distances which are on the butyl group ends of tetrabutylammonium cations. 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^ > 2\s(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^)+(0.0387P)^2^+18.2824P] 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 none _refine_ls_number_reflns 18657 _refine_ls_number_parameters 1055 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1270 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1263 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 0.86042(3) 0.07921(2) 0.54479(3) 0.02298(14) Uani 1 1 d . . . Mo2 Mo 0.81186(3) -0.02280(2) 0.46315(3) 0.02240(14) Uani 1 1 d . . . Mo3 Mo 1.04869(3) 0.10060(2) 0.58314(3) 0.02369(14) Uani 1 1 d . . . Mo4 Mo 0.37724(4) 0.09106(2) 0.96251(3) 0.02851(16) Uani 1 1 d . . . Mo5 Mo 0.41248(4) 0.06065(2) 1.11888(3) 0.03134(17) Uani 1 1 d . . . Mo6 Mo 0.46428(4) 0.03039(2) 0.84231(3) 0.03612(18) Uani 1 1 d . . . Mn1 Mn 1.0000 0.0000 0.5000 0.0173(3) Uani 1 2 d S . . Mn2 Mn 0.5000 0.0000 1.0000 0.0230(3) Uani 1 2 d S . . O1 O 0.7622(2) -0.07222(16) 0.4903(2) 0.0322(12) Uani 1 1 d . . . O2 O 0.7489(3) 0.00839(16) 0.4131(2) 0.0348(12) Uani 1 1 d . . . O3 O 0.8140(2) 0.01491(14) 0.5425(2) 0.0237(10) Uani 1 1 d . . . O4 O 0.7989(2) 0.11396(15) 0.4972(2) 0.0323(12) Uani 1 1 d . . . O5 O 0.8390(3) 0.09401(16) 0.6228(2) 0.0334(12) Uani 1 1 d . . . O6 O 0.9552(2) 0.11501(14) 0.5343(2) 0.0204(10) Uani 1 1 d . . . O7 O 0.9710(2) 0.02955(14) 0.58216(19) 0.0211(10) Uani 1 1 d . . . O8 O 1.0220(3) 0.11462(16) 0.6602(2) 0.0345(12) Uani 1 1 d . . . O9 O 1.1255(2) 0.05204(14) 0.60319(19) 0.0230(10) Uani 1 1 d . . . O10 O 1.1057(3) 0.14826(15) 0.5588(2) 0.0342(12) Uani 1 1 d . . . O11 O 1.0695(2) 0.05524(14) 0.48762(19) 0.0208(10) Uani 1 1 d . . . O12 O 0.9071(2) 0.03667(14) 0.45737(19) 0.0198(10) Uani 1 1 d . . . O13 O 0.4483(3) 0.09512(17) 1.1817(2) 0.0422(13) Uani 1 1 d . . . O14 O 0.4315(3) -0.00481(16) 1.1497(2) 0.0339(12) Uani 1 1 d . . . O15 O 0.3136(3) 0.06117(17) 1.1258(2) 0.0390(13) Uani 1 1 d . . . O16 O 0.5326(3) 0.03597(15) 1.0847(2) 0.0285(11) Uani 1 1 d . . . O17 O 0.4233(3) 0.10502(15) 1.0477(2) 0.0269(11) Uani 1 1 d . . . O18 O 0.3933(3) 0.01618(14) 1.0181(2) 0.0254(11) Uani 1 1 d . . . O19 O 0.2802(3) 0.09305(17) 0.9761(2) 0.0395(13) Uani 1 1 d . . . O20 O 0.3979(3) 0.14511(16) 0.9256(2) 0.0371(12) Uani 1 1 d . . . O21 O 0.3737(3) 0.04651(15) 0.8908(2) 0.0308(11) Uani 1 1 d . . . O22 O 0.5029(3) 0.06100(15) 0.9488(2) 0.0277(11) Uani 1 1 d . . . O23 O 0.4847(3) 0.08488(18) 0.8064(2) 0.0522(15) Uani 1 1 d . . . O24 O 0.4227(3) -0.00456(19) 0.7820(2) 0.0511(15) Uani 1 1 d . . . O25 O 1.1337(3) 0.0839(2) 0.2896(3) 0.0591(17) Uani 1 1 d . . . O26 O 1.2359(3) 0.1626(2) 0.1948(3) 0.0539(15) Uani 1 1 d . . . O27 O 1.1761(3) 0.10059(19) 0.1443(3) 0.0506(15) Uani 1 1 d . . . H27 H 1.2215 0.0897 0.1414 0.076 Uiso 1 1 calc R . . O28 O 0.6431(3) 0.17339(17) 1.0553(3) 0.0424(13) Uani 1 1 d . . . O29 O 0.7139(3) 0.27901(18) 1.0326(3) 0.0445(14) Uani 1 1 d . . . H29 H 0.6823 0.3008 1.0436 0.067 Uiso 1 1 calc R . . O30 O 0.7175(3) 0.2632(2) 1.1396(3) 0.0571(16) Uani 1 1 d . . . N1 N 1.0070(3) 0.08290(19) 0.3144(2) 0.0276(13) Uani 1 1 d . . . H1 H 0.9613 0.0936 0.3003 0.033 Uiso 1 1 calc R . . N2 N 0.6954(3) 0.10514(19) 1.0106(3) 0.0316(14) Uani 1 1 d . . . H2 H 0.7394 0.0926 0.9977 0.038 Uiso 1 1 calc R . . N3 N 0.4095(3) 0.24729(18) 0.1062(3) 0.0301(14) Uani 1 1 d . B . N4 N 0.6495(3) 0.9923(2) 0.6680(3) 0.0305(14) Uani 1 1 d . . . N5 N 0.7289(6) 0.3765(3) 0.2668(4) 0.088(3) Uani 1 1 d . . . N6 N 0.8571(6) 0.1359(4) 0.2740(6) 0.135(5) Uani 1 1 d . . . N7 N 0.8626(6) 0.0583(4) 0.9866(5) 0.096(3) Uani 1 1 d . . . C1 C 1.0078(4) 0.0552(2) 0.3762(3) 0.0230(15) Uani 1 1 d . . . C2 C 1.0660(4) 0.0801(2) 0.4249(3) 0.0273(16) Uani 1 1 d . . . H2A H 1.1183 0.0800 0.4062 0.033 Uiso 1 1 calc R . . H2B H 1.0504 0.1147 0.4314 0.033 Uiso 1 1 calc R . . C3 C 0.9233(4) 0.0611(2) 0.3975(3) 0.0232(15) Uani 1 1 d . . . H3A H 0.9120 0.0966 0.4024 0.028 Uiso 1 1 calc R . . H3B H 0.8881 0.0481 0.3625 0.028 Uiso 1 1 calc R . . C4 C 0.9699(4) -0.0024(2) 0.6389(3) 0.0266(16) Uani 1 1 d . . . H4A H 0.9172 -0.0020 0.6567 0.032 Uiso 1 1 calc R . . H4B H 1.0063 0.0107 0.6730 0.032 Uiso 1 1 calc R . . C5 C 1.0671(4) 0.0940(3) 0.2766(4) 0.0384(19) Uani 1 1 d . . . C6 C 1.0415(4) 0.1182(3) 0.2117(4) 0.047(2) Uani 1 1 d . . . H6A H 1.0397 0.0929 0.1769 0.057 Uiso 1 1 calc R . . H6B H 0.9885 0.1316 0.2156 0.057 Uiso 1 1 calc R . . C7 C 1.0959(5) 0.1593(3) 0.1920(4) 0.043(2) Uani 1 1 d . . . C8 C 1.1775(5) 0.1411(3) 0.1792(4) 0.0368(19) Uani 1 1 d . . . C9 C 1.0998(6) 0.1980(3) 0.2448(4) 0.075(3) Uani 1 1 d . . . H9A H 1.1216 0.1836 0.2853 0.113 Uiso 1 1 calc R . . H9B H 1.0475 0.2104 0.2524 0.113 Uiso 1 1 calc R . . H9C H 1.1329 0.2251 0.2311 0.113 Uiso 1 1 calc R . . C10 C 1.0626(5) 0.1813(3) 0.1276(4) 0.064(3) Uani 1 1 d . . . H10A H 1.0980 0.2066 0.1119 0.096 Uiso 1 1 calc R . . H10B H 1.0118 0.1961 0.1352 0.096 Uiso 1 1 calc R . . H10C H 1.0568 0.1553 0.0947 0.096 Uiso 1 1 calc R . . C11 C 0.6285(4) 0.0719(2) 1.0099(3) 0.0285(16) Uani 1 1 d . . . C12 C 0.5968(4) 0.0696(2) 1.0794(3) 0.0319(17) Uani 1 1 d . . . H12A H 0.6391 0.0593 1.1103 0.038 Uiso 1 1 calc R . . H12B H 0.5798 0.1028 1.0923 0.038 Uiso 1 1 calc R . . C13 C 0.5688(4) 0.0920(2) 0.9587(3) 0.0303(17) Uani 1 1 d . . . H13A H 0.5511 0.1248 0.9730 0.036 Uiso 1 1 calc R . . H13B H 0.5947 0.0962 0.9166 0.036 Uiso 1 1 calc R . . C14 C 0.3371(4) -0.0224(2) 1.0115(4) 0.0327(17) Uani 1 1 d . . . H14A H 0.2964 -0.0123 0.9791 0.039 Uiso 1 1 calc R . . H14B H 0.3120 -0.0270 1.0539 0.039 Uiso 1 1 calc R . . C15 C 0.6970(5) 0.1528(3) 1.0287(4) 0.0390(19) Uani 1 1 d . . . C16 C 0.7706(5) 0.1812(3) 1.0130(4) 0.050(2) Uani 1 1 d . . . H16A H 0.8125 0.1576 1.0038 0.060 Uiso 1 1 calc R . . H16B H 0.7607 0.2012 0.9732 0.060 Uiso 1 1 calc R . . C17 C 0.7975(4) 0.2148(3) 1.0687(4) 0.041(2) Uani 1 1 d . . . C18 C 0.7379(4) 0.2535(3) 1.0856(4) 0.041(2) Uani 1 1 d . . . C19 C 0.8717(5) 0.2410(3) 1.0475(5) 0.063(3) Uani 1 1 d . . . H19A H 0.8588 0.2642 1.0123 0.095 Uiso 1 1 calc R . . H19B H 0.9086 0.2165 1.0319 0.095 Uiso 1 1 calc R . . H19C H 0.8951 0.2587 1.0848 0.095 Uiso 1 1 calc R . . C20 C 0.8151(5) 0.1827(3) 1.1300(4) 0.060(3) Uani 1 1 d . . . H20A H 0.8441 0.2021 1.1628 0.090 Uiso 1 1 calc R . . H20B H 0.8461 0.1541 1.1177 0.090 Uiso 1 1 calc R . . H20C H 0.7662 0.1714 1.1481 0.090 Uiso 1 1 calc R . . C21 C 0.4590(4) 0.2701(2) 0.0532(3) 0.0347(18) Uani 1 1 d . . . H21A H 0.4277 0.2956 0.0302 0.042 Uiso 1 1 calc R . . H21B H 0.5040 0.2867 0.0748 0.042 Uiso 1 1 calc R . . C22 C 0.4890(4) 0.2348(2) 0.0031(4) 0.0372(19) Uani 1 1 d . . . H22A H 0.4453 0.2153 -0.0158 0.045 Uiso 1 1 calc R . . H22B H 0.5264 0.2118 0.0244 0.045 Uiso 1 1 calc R . . C23 C 0.5289(4) 0.2625(3) -0.0516(3) 0.0389(19) Uani 1 1 d . . . H23A H 0.4894 0.2814 -0.0772 0.047 Uiso 1 1 calc R . . H23B H 0.5663 0.2863 -0.0319 0.047 Uiso 1 1 calc R . . C24 C 0.5713(5) 0.2293(3) -0.0971(4) 0.055(2) Uani 1 1 d . . . H24A H 0.6151 0.2137 -0.0734 0.082 Uiso 1 1 calc R . . H24B H 0.5908 0.2486 -0.1336 0.082 Uiso 1 1 calc R . . H24C H 0.5358 0.2038 -0.1140 0.082 Uiso 1 1 calc R . . C25 C 0.3389(4) 0.2220(2) 0.0759(4) 0.0338(18) Uani 1 1 d . . . H25A H 0.3567 0.1948 0.0480 0.041 Uiso 1 1 calc R . . H25B H 0.3089 0.2073 0.1114 0.041 Uiso 1 1 calc R . . C26 C 0.2859(5) 0.2543(3) 0.0357(4) 0.054(2) Uani 1 1 d . . . H26A H 0.2625 0.2791 0.0645 0.065 Uiso 1 1 calc R . . H26B H 0.3166 0.2720 0.0031 0.065 Uiso 1 1 calc R . . C27 C 0.2226(5) 0.2262(3) 0.0009(4) 0.062(3) Uani 1 1 d . . . H27A H 0.1935 0.2073 0.0333 0.074 Uiso 1 1 calc R . . H27B H 0.2460 0.2025 -0.0293 0.074 Uiso 1 1 calc R . . C28 C 0.1667(6) 0.2589(4) -0.0374(5) 0.098(4) Uani 1 1 d . . . H28A H 0.1451 0.2835 -0.0081 0.148 Uiso 1 1 calc R . . H28B H 0.1246 0.2389 -0.0565 0.148 Uiso 1 1 calc R . . H28C H 0.1942 0.2754 -0.0723 0.148 Uiso 1 1 calc R . . C29 C 0.3861(4) 0.2901(2) 0.1492(3) 0.0322(17) Uani 1 1 d . . . H29A H 0.4338 0.3079 0.1635 0.039 Uiso 1 1 calc R . . H29B H 0.3542 0.3131 0.1222 0.039 Uiso 1 1 calc R . . C30 C 0.3417(5) 0.2772(3) 0.2089(3) 0.0390(19) Uani 1 1 d . . . H30A H 0.3745 0.2568 0.2387 0.047 Uiso 1 1 calc R . . H30B H 0.2950 0.2579 0.1959 0.047 Uiso 1 1 calc R . . C31 C 0.3175(5) 0.3237(3) 0.2440(4) 0.049(2) Uani 1 1 d . . . H31A H 0.3646 0.3432 0.2553 0.059 Uiso 1 1 calc R . . H31B H 0.2846 0.3437 0.2138 0.059 Uiso 1 1 calc R . . C32 C 0.2739(6) 0.3144(3) 0.3053(4) 0.073(3) Uani 1 1 d . . . H32A H 0.2278 0.2945 0.2948 0.109 Uiso 1 1 calc R . . H32B H 0.2581 0.3459 0.3240 0.109 Uiso 1 1 calc R . . H32C H 0.3075 0.2968 0.3369 0.109 Uiso 1 1 calc R . . C33 C 0.4563(4) 0.2094(2) 0.1444(4) 0.0369(19) Uani 1 1 d . . . H33A H 0.4704 0.1826 0.1142 0.044 Uiso 1 1 calc R A 1 H33B H 0.4228 0.1949 0.1778 0.044 Uiso 1 1 calc R A 1 C34 C 0.5300(5) 0.2283(3) 0.1783(4) 0.058(2) Uani 1 1 d . B 1 H34A H 0.5675 0.2382 0.1452 0.069 Uiso 1 1 calc R B 1 H34B H 0.5178 0.2577 0.2047 0.069 Uiso 1 1 calc R B 1 C35 C 0.5658(6) 0.1894(4) 0.2221(5) 0.079(3) Uani 1 1 d D B 1 H35A H 0.5644 0.1573 0.1991 0.095 Uiso 1 1 calc R B 1 H35B H 0.6208 0.1977 0.2321 0.095 Uiso 1 1 calc R B 1 C36 C 0.5247(8) 0.1855(4) 0.2819(6) 0.066(4) Uani 0.70 1 d PD B 1 H36A H 0.5154 0.2184 0.2993 0.099 Uiso 1 1 calc R B 1 H36B H 0.5558 0.1665 0.3138 0.099 Uiso 1 1 calc R B 1 H36C H 0.4750 0.1689 0.2734 0.099 Uiso 1 1 calc R B 1 C36' C 0.6262(15) 0.1925(11) 0.2733(13) 0.065(9) Uiso 0.30 1 d PD C 2 C37 C 0.6858(4) 1.0003(3) 0.7358(3) 0.0379(19) Uani 1 1 d . . . H37A H 0.6551 1.0254 0.7586 0.045 Uiso 1 1 calc R . . H37B H 0.6821 0.9692 0.7607 0.045 Uiso 1 1 calc R . . C38 C 0.7701(4) 1.0165(3) 0.7368(4) 0.045(2) Uani 1 1 d . . . H38A H 0.8026 0.9893 0.7207 0.054 Uiso 1 1 calc R . . H38B H 0.7757 1.0448 0.7070 0.054 Uiso 1 1 calc R . . C39 C 0.7980(5) 1.0307(3) 0.8036(4) 0.054(2) Uani 1 1 d . . . H39A H 0.7872 1.0037 0.8343 0.065 Uiso 1 1 calc R . . H39B H 0.7690 1.0601 0.8178 0.065 Uiso 1 1 calc R . . C40 C 0.8853(5) 1.0421(3) 0.8068(4) 0.062(3) Uani 1 1 d . . . H40A H 0.9147 1.0115 0.8033 0.093 Uiso 1 1 calc R . . H40B H 0.8988 1.0581 0.8485 0.093 Uiso 1 1 calc R . . H40C H 0.8981 1.0641 0.7708 0.093 Uiso 1 1 calc R . . C41 C 0.6923(4) 0.9513(2) 0.6339(4) 0.0362(19) Uani 1 1 d . . . H41A H 0.6750 0.9510 0.5873 0.043 Uiso 1 1 calc R . . H41B H 0.7484 0.9591 0.6356 0.043 Uiso 1 1 calc R . . C42 C 0.6812(4) 0.9005(3) 0.6617(4) 0.045(2) Uani 1 1 d . . . H42A H 0.6251 0.8938 0.6656 0.054 Uiso 1 1 calc R . . H42B H 0.7058 0.8987 0.7060 0.054 Uiso 1 1 calc R . . C43 C 0.7170(5) 0.8613(3) 0.6179(5) 0.062(3) Uani 1 1 d . . . H43A H 0.6969 0.8662 0.5726 0.074 Uiso 1 1 calc R . . H43B H 0.7739 0.8664 0.6181 0.074 Uiso 1 1 calc R . . C44 C 0.7018(6) 0.8103(3) 0.6369(5) 0.082(3) Uani 1 1 d . . . H44A H 0.7191 0.8053 0.6825 0.123 Uiso 1 1 calc R . . H44B H 0.7302 0.7880 0.6086 0.123 Uiso 1 1 calc R . . H44C H 0.6461 0.8036 0.6323 0.123 Uiso 1 1 calc R . . C45 C 0.5649(4) 0.9800(3) 0.6766(3) 0.0355(18) Uani 1 1 d . . . H45A H 0.5386 1.0091 0.6946 0.043 Uiso 1 1 calc R . . H45B H 0.5614 0.9531 0.7090 0.043 Uiso 1 1 calc R . . C46 C 0.5220(4) 0.9644(4) 0.6138(4) 0.060(3) Uani 1 1 d . . . H46A H 0.5200 0.9925 0.5832 0.072 Uiso 1 1 calc R . . H46B H 0.5513 0.9376 0.5931 0.072 Uiso 1 1 calc R . . C47 C 0.4412(4) 0.9471(3) 0.6250(4) 0.050(2) Uani 1 1 d . . . H47A H 0.4104 0.9747 0.6421 0.060 Uiso 1 1 calc R . . H47B H 0.4427 0.9208 0.6584 0.060 Uiso 1 1 calc R . . C48 C 0.4021(6) 0.9278(5) 0.5627(5) 0.116(5) Uani 1 1 d . . . H48A H 0.4208 0.9463 0.5252 0.174 Uiso 1 1 calc R . . H48B H 0.3458 0.9319 0.5651 0.174 Uiso 1 1 calc R . . H48C H 0.4145 0.8929 0.5575 0.174 Uiso 1 1 calc R . . C49 C 0.6576(4) 1.0385(2) 0.6275(3) 0.0347(18) Uani 1 1 d . . . H49A H 0.6271 1.0341 0.5861 0.042 Uiso 1 1 calc R . . H49B H 0.7127 1.0420 0.6162 0.042 Uiso 1 1 calc R . . C50 C 0.6318(4) 1.0858(3) 0.6592(4) 0.0401(19) Uani 1 1 d . . . H50A H 0.5786 1.0816 0.6751 0.048 Uiso 1 1 calc R . . H50B H 0.6666 1.0931 0.6973 0.048 Uiso 1 1 calc R . . C51 C 0.6329(5) 1.1283(3) 0.6119(4) 0.050(2) Uani 1 1 d . . . H51A H 0.5991 1.1204 0.5734 0.060 Uiso 1 1 calc R . . H51B H 0.6864 1.1328 0.5967 0.060 Uiso 1 1 calc R . . C52 C 0.6056(6) 1.1760(3) 0.6420(5) 0.076(3) Uani 1 1 d . . . H52A H 0.5530 1.1716 0.6580 0.114 Uiso 1 1 calc R . . H52B H 0.6052 1.2021 0.6090 0.114 Uiso 1 1 calc R . . H52C H 0.6408 1.1851 0.6785 0.114 Uiso 1 1 calc R . . C53 C 0.7478(7) 0.3744(4) 0.1969(5) 0.087(4) Uani 1 1 d . . . H53A H 0.7047 0.3897 0.1712 0.105 Uiso 1 1 calc R . . H53B H 0.7505 0.3394 0.1837 0.105 Uiso 1 1 calc R . . C54 C 0.8227(8) 0.3992(4) 0.1786(5) 0.089(4) Uani 1 1 d . . . H54A H 0.8622 0.3947 0.2143 0.107 Uiso 1 1 calc R . . H54B H 0.8137 0.4349 0.1728 0.107 Uiso 1 1 calc R . . C55 C 0.8525(7) 0.3773(4) 0.1155(6) 0.095(4) Uani 1 1 d . . . H55A H 0.8755 0.3446 0.1249 0.114 Uiso 1 1 calc R . . H55B H 0.8084 0.3727 0.0840 0.114 Uiso 1 1 calc R . . C56 C 0.9121(6) 0.4093(5) 0.0852(6) 0.114(5) Uani 1 1 d . . . H56A H 0.8879 0.4402 0.0708 0.171 Uiso 1 1 calc R . . H56B H 0.9336 0.3924 0.0476 0.171 Uiso 1 1 calc R . . H56C H 0.9539 0.4163 0.1175 0.171 Uiso 1 1 calc R . . C57 C 0.7360(7) 0.4295(3) 0.2910(5) 0.095(4) Uani 1 1 d . E . H57A H 0.7886 0.4418 0.2820 0.114 Uiso 1 1 calc R . . H57B H 0.7301 0.4299 0.3390 0.114 Uiso 1 1 calc R . . C58 C 0.6762(7) 0.4645(4) 0.2597(5) 0.101(4) Uani 1 1 d . . . H58A H 0.6232 0.4545 0.2715 0.122 Uiso 1 1 calc R D 1 H58B H 0.6794 0.4634 0.2115 0.122 Uiso 1 1 calc R D 1 C59 C 0.6934(8) 0.5165(5) 0.2845(6) 0.119(5) Uiso 1 1 d D E 1 H59A H 0.7495 0.5237 0.2819 0.143 Uiso 1 1 calc R E 1 H59B H 0.6644 0.5409 0.2574 0.143 Uiso 1 1 calc R E 1 C60 C 0.6698(10) 0.5196(7) 0.3516(8) 0.126(7) Uiso 0.70 1 d PD E 1 H60A H 0.6193 0.5036 0.3557 0.190 Uiso 1 1 calc R E 1 H60B H 0.6658 0.5542 0.3644 0.190 Uiso 1 1 calc R E 1 H60C H 0.7084 0.5031 0.3801 0.190 Uiso 1 1 calc R E 1 C60' C 0.757(2) 0.5496(15) 0.259(2) 0.126(16) Uiso 0.30 1 d PD F 2 C61 C 0.6474(6) 0.3555(4) 0.2721(6) 0.089(4) Uani 1 1 d . . . H61A H 0.6121 0.3740 0.2420 0.107 Uiso 1 1 calc R . . H61B H 0.6479 0.3210 0.2569 0.107 Uiso 1 1 calc R . . C62 C 0.6141(7) 0.3566(5) 0.3391(6) 0.105(4) Uani 1 1 d . . . H62A H 0.6125 0.3910 0.3548 0.126 Uiso 1 1 calc R . . H62B H 0.6482 0.3377 0.3697 0.126 Uiso 1 1 calc R . . C63 C 0.5323(7) 0.3349(5) 0.3384(6) 0.107(4) Uani 1 1 d . . . H63A H 0.4998 0.3522 0.3050 0.129 Uiso 1 1 calc R . . H63B H 0.5350 0.2999 0.3256 0.129 Uiso 1 1 calc R . . C64 C 0.4942(8) 0.3386(5) 0.4028(7) 0.144(6) Uani 1 1 d . . . H64A H 0.5273 0.3231 0.4367 0.216 Uiso 1 1 calc R . . H64B H 0.4439 0.3217 0.4002 0.216 Uiso 1 1 calc R . . H64C H 0.4863 0.3732 0.4137 0.216 Uiso 1 1 calc R . . C65 C 0.7875(6) 0.3466(3) 0.3078(5) 0.083(4) Uani 1 1 d . H . H65A H 0.7791 0.3532 0.3545 0.099 Uiso 1 1 calc R . . H65B H 0.8404 0.3580 0.2980 0.099 Uiso 1 1 calc R . . C66 C 0.7831(8) 0.2903(4) 0.2962(6) 0.124(5) Uani 1 1 d . . . H66A H 0.7371 0.2769 0.3179 0.149 Uiso 1 1 calc R G 1 H66B H 0.7769 0.2837 0.2488 0.149 Uiso 1 1 calc R G 1 C67 C 0.8558(8) 0.2647(4) 0.3230(7) 0.145(8) Uani 1 1 d . H 1 H67A H 0.8499 0.2285 0.3217 0.175 Uiso 1 1 calc R H 1 H67B H 0.8685 0.2751 0.3684 0.175 Uiso 1 1 calc R H 1 C68 C 0.9181(14) 0.2821(9) 0.2758(12) 0.160(12) Uiso 0.60 1 d P H 1 H68A H 0.8928 0.2959 0.2363 0.240 Uiso 1 1 calc R H 1 H68B H 0.9507 0.2542 0.2638 0.240 Uiso 1 1 calc R H 1 H68C H 0.9504 0.3074 0.2972 0.240 Uiso 1 1 calc R H 1 C68' C 0.848(2) 0.2082(17) 0.328(2) 0.170(17) Uiso 0.40 1 d P I 2 C69 C 0.7972(11) 0.1272(6) 0.2954(8) 0.135(6) Uiso 1 1 d . . . C70 C 0.7166(11) 0.1101(7) 0.3178(9) 0.210(8) Uiso 1 1 d . . . H70A H 0.7128 0.1156 0.3649 0.315 Uiso 1 1 calc R . . H70B H 0.7099 0.0750 0.3083 0.315 Uiso 1 1 calc R . . H70C H 0.6759 0.1289 0.2944 0.315 Uiso 1 1 calc R . . C71 C 0.8739(6) 0.0175(5) 0.9844(5) 0.075(3) Uani 1 1 d . . . C72 C 0.8839(7) -0.0368(4) 0.9822(6) 0.107(4) Uani 1 1 d . . . H72A H 0.8344 -0.0528 0.9910 0.161 Uiso 1 1 calc R . . H72B H 0.9230 -0.0469 1.0153 0.161 Uiso 1 1 calc R . . H72C H 0.9008 -0.0466 0.9388 0.161 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 0.0202(3) 0.0209(3) 0.0280(3) -0.0011(3) 0.0041(3) 0.0009(3) Mo2 0.0160(3) 0.0245(3) 0.0267(3) -0.0003(3) 0.0009(3) -0.0025(3) Mo3 0.0215(3) 0.0207(3) 0.0286(3) -0.0035(3) -0.0024(3) -0.0002(3) Mo4 0.0355(4) 0.0232(3) 0.0269(3) 0.0023(3) 0.0022(3) 0.0096(3) Mo5 0.0448(4) 0.0269(3) 0.0232(3) 0.0036(3) 0.0145(3) 0.0108(3) Mo6 0.0525(5) 0.0361(4) 0.0202(3) 0.0077(3) 0.0091(3) 0.0158(3) Mn1 0.0156(7) 0.0176(7) 0.0190(7) 0.0023(6) 0.0017(6) -0.0013(6) Mn2 0.0309(9) 0.0205(7) 0.0181(8) 0.0040(6) 0.0067(6) 0.0079(7) O1 0.023(3) 0.030(3) 0.044(3) -0.002(2) 0.005(2) -0.014(2) O2 0.025(3) 0.036(3) 0.042(3) 0.002(2) -0.008(2) 0.006(2) O3 0.018(2) 0.024(2) 0.029(3) 0.000(2) 0.009(2) -0.001(2) O4 0.023(3) 0.029(3) 0.045(3) 0.008(2) 0.003(2) 0.005(2) O5 0.037(3) 0.030(3) 0.033(3) -0.005(2) 0.010(2) -0.003(2) O6 0.020(2) 0.016(2) 0.025(2) 0.0001(19) 0.0004(19) 0.0028(19) O7 0.022(2) 0.021(2) 0.020(2) 0.0079(19) -0.0027(19) 0.001(2) O8 0.036(3) 0.036(3) 0.032(3) -0.012(2) -0.002(2) 0.002(2) O9 0.025(3) 0.022(2) 0.022(2) 0.0010(19) 0.000(2) -0.004(2) O10 0.028(3) 0.021(2) 0.053(3) 0.003(2) -0.007(2) -0.005(2) O11 0.024(3) 0.018(2) 0.019(2) 0.0045(19) -0.0001(19) -0.002(2) O12 0.024(2) 0.017(2) 0.018(2) 0.0037(19) 0.0036(19) -0.0031(19) O13 0.067(4) 0.033(3) 0.027(3) -0.002(2) 0.014(3) 0.012(3) O14 0.047(3) 0.034(3) 0.021(3) 0.010(2) 0.018(2) 0.012(2) O15 0.046(3) 0.040(3) 0.031(3) 0.008(2) 0.019(2) 0.012(3) O16 0.035(3) 0.023(2) 0.029(3) 0.001(2) 0.013(2) 0.001(2) O17 0.038(3) 0.023(2) 0.020(2) 0.002(2) 0.010(2) 0.008(2) O18 0.035(3) 0.021(2) 0.021(2) 0.0009(19) 0.008(2) 0.001(2) O19 0.037(3) 0.035(3) 0.047(3) -0.008(2) 0.002(3) 0.010(2) O20 0.051(3) 0.029(3) 0.031(3) 0.009(2) -0.004(2) 0.006(2) O21 0.040(3) 0.029(3) 0.024(3) -0.003(2) 0.003(2) 0.009(2) O22 0.036(3) 0.023(2) 0.024(3) -0.001(2) 0.008(2) 0.004(2) O23 0.069(4) 0.046(3) 0.043(3) 0.022(3) 0.016(3) 0.019(3) O24 0.075(4) 0.057(3) 0.022(3) -0.008(3) 0.007(3) 0.019(3) O25 0.025(3) 0.106(5) 0.047(3) 0.044(3) 0.003(3) 0.002(3) O26 0.051(4) 0.054(4) 0.058(4) 0.002(3) 0.010(3) -0.020(3) O27 0.041(3) 0.046(3) 0.065(4) -0.007(3) -0.003(3) 0.009(3) O28 0.038(3) 0.029(3) 0.061(4) -0.005(3) 0.016(3) 0.001(2) O29 0.040(4) 0.037(3) 0.057(4) 0.001(3) -0.004(3) 0.012(3) O30 0.076(5) 0.053(4) 0.043(4) -0.010(3) 0.001(3) -0.002(3) N1 0.019(3) 0.038(3) 0.025(3) 0.015(3) 0.003(3) 0.000(3) N2 0.026(3) 0.028(3) 0.042(4) -0.007(3) 0.010(3) 0.005(3) N3 0.033(4) 0.015(3) 0.043(4) 0.001(3) 0.005(3) -0.002(3) N4 0.030(4) 0.040(3) 0.023(3) 0.011(3) 0.015(3) 0.008(3) N5 0.127(9) 0.076(6) 0.058(6) -0.013(5) -0.062(6) 0.036(6) N6 0.082(8) 0.140(10) 0.183(12) 0.068(9) 0.022(8) 0.027(7) N7 0.093(8) 0.078(7) 0.119(9) -0.013(6) 0.020(6) 0.011(6) C1 0.024(4) 0.022(3) 0.022(4) 0.008(3) 0.001(3) -0.003(3) C2 0.025(4) 0.029(4) 0.027(4) 0.009(3) 0.001(3) -0.005(3) C3 0.025(4) 0.028(4) 0.018(4) 0.005(3) 0.004(3) 0.002(3) C4 0.022(4) 0.032(4) 0.025(4) 0.010(3) 0.002(3) 0.003(3) C5 0.028(5) 0.052(5) 0.035(5) 0.019(4) 0.001(4) -0.001(4) C6 0.030(5) 0.074(6) 0.037(5) 0.038(4) 0.005(4) 0.006(4) C7 0.048(5) 0.042(5) 0.040(5) 0.015(4) 0.012(4) 0.013(4) C8 0.044(5) 0.032(4) 0.035(5) 0.006(4) 0.004(4) 0.002(4) C9 0.097(8) 0.063(6) 0.067(7) 0.004(5) 0.012(6) 0.021(6) C10 0.063(6) 0.065(6) 0.064(6) 0.031(5) 0.010(5) 0.017(5) C11 0.033(4) 0.018(3) 0.034(4) -0.001(3) 0.006(3) -0.002(3) C12 0.037(4) 0.029(4) 0.031(4) 0.003(3) 0.009(3) 0.002(3) C13 0.035(4) 0.030(4) 0.026(4) 0.006(3) 0.005(3) 0.006(3) C14 0.027(4) 0.030(4) 0.040(5) -0.004(3) 0.006(3) 0.000(3) C15 0.039(5) 0.035(4) 0.044(5) -0.004(4) 0.006(4) 0.005(4) C16 0.048(5) 0.053(5) 0.048(5) -0.012(4) 0.005(4) 0.005(4) C17 0.031(5) 0.036(4) 0.056(5) 0.007(4) -0.007(4) 0.004(4) C18 0.034(5) 0.033(4) 0.057(6) -0.004(4) -0.012(4) -0.003(4) C19 0.046(6) 0.054(6) 0.089(7) 0.004(5) -0.003(5) 0.004(5) C20 0.060(6) 0.060(6) 0.058(6) 0.007(5) -0.013(5) 0.016(5) C21 0.036(5) 0.032(4) 0.037(5) 0.000(3) 0.007(4) -0.004(3) C22 0.033(5) 0.031(4) 0.049(5) -0.001(4) 0.016(4) 0.003(3) C23 0.040(5) 0.039(4) 0.039(5) 0.001(4) 0.005(4) -0.006(4) C24 0.056(6) 0.060(6) 0.049(6) 0.004(5) 0.015(5) 0.010(5) C25 0.032(4) 0.031(4) 0.039(5) -0.002(3) 0.004(4) -0.011(3) C26 0.053(6) 0.047(5) 0.061(6) 0.006(4) -0.020(5) 0.005(4) C27 0.036(5) 0.081(7) 0.067(6) -0.018(5) -0.014(5) -0.004(5) C28 0.077(8) 0.117(9) 0.098(9) -0.033(7) -0.049(7) 0.028(7) C29 0.036(4) 0.020(4) 0.041(5) 0.001(3) 0.004(4) -0.003(3) C30 0.053(5) 0.034(4) 0.030(4) 0.000(4) 0.007(4) -0.003(4) C31 0.061(6) 0.037(5) 0.049(5) -0.005(4) 0.009(4) 0.006(4) C32 0.122(9) 0.048(5) 0.049(6) -0.004(5) 0.029(6) 0.004(6) C33 0.044(5) 0.031(4) 0.035(5) -0.007(3) -0.003(4) 0.010(4) C34 0.053(6) 0.061(6) 0.059(6) -0.009(5) -0.012(5) 0.015(5) C35 0.072(7) 0.101(8) 0.064(7) -0.009(6) -0.019(6) 0.032(6) C36 0.088(11) 0.055(8) 0.054(9) 0.012(7) -0.013(8) 0.010(8) C37 0.031(4) 0.057(5) 0.026(4) 0.016(4) 0.006(3) 0.005(4) C38 0.031(5) 0.069(6) 0.035(5) 0.025(4) 0.000(4) 0.000(4) C39 0.048(6) 0.052(5) 0.062(6) 0.006(5) 0.006(5) -0.002(5) C40 0.048(6) 0.063(6) 0.075(7) 0.016(5) -0.010(5) -0.006(5) C41 0.026(4) 0.044(4) 0.039(5) 0.010(4) 0.018(4) 0.006(4) C42 0.035(5) 0.040(5) 0.060(6) 0.021(4) 0.014(4) -0.004(4) C43 0.048(6) 0.043(5) 0.096(8) 0.018(5) 0.025(5) 0.006(4) C44 0.099(9) 0.050(6) 0.098(8) 0.001(6) 0.025(7) -0.002(6) C45 0.029(4) 0.056(5) 0.023(4) 0.011(4) 0.011(3) 0.004(4) C46 0.035(5) 0.110(8) 0.034(5) -0.006(5) 0.004(4) 0.021(5) C47 0.031(5) 0.067(6) 0.053(5) -0.014(5) 0.001(4) 0.010(4) C48 0.063(7) 0.180(12) 0.104(9) -0.105(9) -0.030(7) 0.046(8) C49 0.035(4) 0.041(4) 0.029(4) 0.013(4) 0.012(3) 0.016(4) C50 0.038(5) 0.044(5) 0.039(5) 0.000(4) 0.005(4) 0.006(4) C51 0.060(6) 0.041(5) 0.051(5) 0.008(4) 0.009(5) 0.007(4) C52 0.082(8) 0.045(5) 0.100(8) -0.005(5) 0.004(6) 0.022(5) C53 0.103(10) 0.067(7) 0.088(9) -0.013(6) -0.057(7) 0.015(7) C54 0.131(11) 0.065(7) 0.069(8) -0.012(6) -0.050(8) 0.023(8) C55 0.085(9) 0.076(8) 0.118(10) 0.012(8) -0.063(8) 0.004(7) C56 0.060(8) 0.120(11) 0.158(13) 0.004(9) -0.044(8) 0.000(8) C57 0.153(11) 0.064(7) 0.065(7) -0.020(6) -0.068(7) 0.035(7) C58 0.152(11) 0.073(7) 0.075(8) -0.013(6) -0.066(8) 0.037(8) C61 0.088(9) 0.083(8) 0.094(9) -0.001(7) -0.061(7) 0.017(7) C62 0.123(12) 0.113(10) 0.077(9) 0.003(8) -0.053(8) 0.019(9) C63 0.098(10) 0.110(10) 0.111(11) -0.022(9) -0.049(9) 0.015(8) C64 0.147(14) 0.161(14) 0.122(13) 0.006(11) -0.016(11) 0.055(12) C65 0.113(9) 0.069(7) 0.062(6) -0.020(5) -0.061(6) 0.035(6) C66 0.183(14) 0.075(8) 0.109(10) -0.027(7) -0.090(10) 0.025(9) C67 0.198(15) 0.064(7) 0.165(14) -0.072(8) -0.149(13) 0.072(9) C71 0.058(7) 0.085(8) 0.083(8) -0.021(7) 0.004(6) -0.005(7) C72 0.099(10) 0.093(9) 0.131(11) -0.035(8) 0.007(8) -0.005(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O5 1.699(4) . ? Mo1 O4 1.704(4) . ? Mo1 O6 1.921(4) . ? Mo1 O3 1.923(4) . ? Mo1 O12 2.298(4) . ? Mo1 O7 2.441(4) . ? Mo2 O2 1.696(4) . ? Mo2 O1 1.697(4) . ? Mo2 O3 1.922(4) . ? Mo2 O9 1.932(4) 3_756 ? Mo2 O12 2.310(4) . ? Mo2 O11 2.419(4) 3_756 ? Mo3 O8 1.701(4) . ? Mo3 O10 1.711(4) . ? Mo3 O9 1.906(4) . ? Mo3 O6 1.911(4) . ? Mo3 O11 2.349(4) . ? Mo3 O7 2.351(4) . ? Mo4 O20 1.696(4) . ? Mo4 O19 1.706(5) . ? Mo4 O21 1.904(4) . ? Mo4 O17 1.931(4) . ? Mo4 O22 2.341(4) . ? Mo4 O18 2.346(4) . ? Mo5 O13 1.692(5) . ? Mo5 O15 1.716(5) . ? Mo5 O17 1.906(4) . ? Mo5 O14 1.914(4) . ? Mo5 O16 2.307(4) . ? Mo5 O18 2.405(4) . ? Mo6 O23 1.696(5) . ? Mo6 O24 1.699(5) . ? Mo6 O21 1.926(4) . ? Mo6 O14 1.929(5) 3_657 ? Mo6 O16 2.343(4) 3_657 ? Mo6 O22 2.408(4) . ? Mn1 O11 1.943(4) 3_756 ? Mn1 O11 1.943(4) . ? Mn1 O7 1.944(4) . ? Mn1 O7 1.944(4) 3_756 ? Mn1 O12 2.058(4) 3_756 ? Mn1 O12 2.058(4) . ? Mn2 O18 1.938(4) 3_657 ? Mn2 O18 1.938(4) . ? Mn2 O22 1.964(4) 3_657 ? Mn2 O22 1.964(4) . ? Mn2 O16 2.055(4) 3_657 ? Mn2 O16 2.055(4) . ? O7 C4 1.451(7) . ? O9 Mo2 1.932(4) 3_756 ? O11 C2 1.451(7) . ? O11 Mo2 2.419(4) 3_756 ? O12 C3 1.431(7) . ? O14 Mo6 1.929(5) 3_657 ? O16 C12 1.442(8) . ? O16 Mo6 2.343(4) 3_657 ? O18 C14 1.433(7) . ? O22 C13 1.425(8) . ? O25 C5 1.204(8) . ? O26 C8 1.198(8) . ? O27 C8 1.313(8) . ? O28 C15 1.226(8) . ? O29 C18 1.343(9) . ? O30 C18 1.200(9) . ? N1 C5 1.346(8) . ? N1 C1 1.472(7) . ? N2 C15 1.350(8) . ? N2 C11 1.465(8) . ? N3 C33 1.512(8) . ? N3 C25 1.514(8) . ? N3 C29 1.523(8) . ? N3 C21 1.531(8) . ? N4 C45 1.512(8) . ? N4 C49 1.514(8) . ? N4 C41 1.519(8) . ? N4 C37 1.520(8) . ? N5 C53 1.479(13) . ? N5 C61 1.524(13) . ? N5 C65 1.527(10) . ? N5 C57 1.528(11) . ? N6 C69 1.160(17) . ? N7 C71 1.129(12) . ? C1 C4 1.522(8) 3_756 ? C1 C3 1.542(9) . ? C1 C2 1.548(8) . ? C4 C1 1.522(8) 3_756 ? C5 C6 1.534(9) . ? C6 C7 1.521(10) . ? C7 C9 1.509(11) . ? C7 C8 1.523(10) . ? C7 C10 1.544(10) . ? C11 C14 1.540(9) 3_657 ? C11 C12 1.541(9) . ? C11 C13 1.545(9) . ? C14 C11 1.540(9) 3_657 ? C15 C16 1.527(10) . ? C16 C17 1.522(10) . ? C17 C18 1.517(10) . ? C17 C19 1.538(11) . ? C17 C20 1.552(10) . ? C21 C22 1.509(9) . ? C22 C23 1.531(9) . ? C23 C24 1.504(10) . ? C25 C26 1.497(10) . ? C26 C27 1.494(10) . ? C27 C28 1.512(12) . ? C29 C30 1.504(9) . ? C30 C31 1.519(9) . ? C31 C32 1.504(10) . ? C33 C34 1.519(10) . ? C34 C35 1.507(11) . ? C35 C36 1.439(12) . ? C37 C38 1.518(9) . ? C38 C39 1.487(10) . ? C39 C40 1.535(11) . ? C41 C42 1.511(9) . ? C42 C43 1.535(10) . ? C43 C44 1.466(11) . ? C45 C46 1.524(10) . ? C46 C47 1.494(10) . ? C47 C48 1.519(11) . ? C49 C50 1.514(9) . ? C50 C51 1.509(10) . ? C51 C52 1.517(10) . ? C53 C54 1.513(14) . ? C54 C55 1.527(14) . ? C55 C56 1.495(14) . ? C57 C58 1.529(12) . ? C58 C59 1.530(14) . ? C59 C60 1.446(14) . ? C61 C62 1.502(14) . ? C62 C63 1.529(15) . ? C63 C64 1.494(15) . ? C65 C66 1.551(13) . ? C66 C67 1.521(14) . ? C67 C68 1.54(2) . ? C69 C70 1.55(2) . ? C71 C72 1.490(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mo1 O4 104.9(2) . . ? O5 Mo1 O6 101.30(19) . . ? O4 Mo1 O6 99.83(19) . . ? O5 Mo1 O3 97.80(19) . . ? O4 Mo1 O3 103.9(2) . . ? O6 Mo1 O3 144.40(17) . . ? O5 Mo1 O12 160.60(18) . . ? O4 Mo1 O12 93.45(18) . . ? O6 Mo1 O12 81.26(15) . . ? O3 Mo1 O12 71.25(15) . . ? O5 Mo1 O7 91.54(18) . . ? O4 Mo1 O7 162.27(18) . . ? O6 Mo1 O7 69.90(15) . . ? O3 Mo1 O7 79.88(15) . . ? O12 Mo1 O7 71.11(14) . . ? O2 Mo2 O1 105.9(2) . . ? O2 Mo2 O3 103.8(2) . . ? O1 Mo2 O3 98.20(19) . . ? O2 Mo2 O9 98.2(2) . 3_756 ? O1 Mo2 O9 101.71(19) . 3_756 ? O3 Mo2 O9 144.86(17) . 3_756 ? O2 Mo2 O12 93.48(18) . . ? O1 Mo2 O12 159.76(18) . . ? O3 Mo2 O12 70.99(15) . . ? O9 Mo2 O12 80.73(15) 3_756 . ? O2 Mo2 O11 161.94(19) . 3_756 ? O1 Mo2 O11 90.21(18) . 3_756 ? O3 Mo2 O11 81.28(15) . 3_756 ? O9 Mo2 O11 70.06(15) 3_756 3_756 ? O12 Mo2 O11 71.56(13) . 3_756 ? O8 Mo3 O10 105.9(2) . . ? O8 Mo3 O9 99.3(2) . . ? O10 Mo3 O9 100.73(19) . . ? O8 Mo3 O6 101.1(2) . . ? O10 Mo3 O6 100.07(19) . . ? O9 Mo3 O6 145.47(17) . . ? O8 Mo3 O11 160.53(18) . . ? O10 Mo3 O11 92.97(19) . . ? O9 Mo3 O11 72.08(15) . . ? O6 Mo3 O11 79.61(15) . . ? O8 Mo3 O7 91.26(18) . . ? O10 Mo3 O7 162.35(19) . . ? O9 Mo3 O7 79.85(15) . . ? O6 Mo3 O7 72.15(15) . . ? O11 Mo3 O7 70.28(14) . . ? O20 Mo4 O19 105.4(2) . . ? O20 Mo4 O21 102.1(2) . . ? O19 Mo4 O21 97.9(2) . . ? O20 Mo4 O17 98.4(2) . . ? O19 Mo4 O17 103.0(2) . . ? O21 Mo4 O17 145.52(18) . . ? O20 Mo4 O22 92.37(19) . . ? O19 Mo4 O22 161.27(19) . . ? O21 Mo4 O22 72.08(17) . . ? O17 Mo4 O22 79.70(16) . . ? O20 Mo4 O18 161.0(2) . . ? O19 Mo4 O18 92.88(19) . . ? O21 Mo4 O18 79.76(16) . . ? O17 Mo4 O18 72.15(16) . . ? O22 Mo4 O18 70.07(15) . . ? O13 Mo5 O15 105.9(2) . . ? O13 Mo5 O17 100.8(2) . . ? O15 Mo5 O17 100.3(2) . . ? O13 Mo5 O14 102.1(2) . . ? O15 Mo5 O14 98.1(2) . . ? O17 Mo5 O14 145.23(17) . . ? O13 Mo5 O16 94.7(2) . . ? O15 Mo5 O16 158.7(2) . . ? O17 Mo5 O16 80.94(17) . . ? O14 Mo5 O16 71.51(17) . . ? O13 Mo5 O18 165.3(2) . . ? O15 Mo5 O18 87.96(19) . . ? O17 Mo5 O18 71.14(16) . . ? O14 Mo5 O18 80.34(16) . . ? O16 Mo5 O18 72.19(15) . . ? O23 Mo6 O24 105.2(3) . . ? O23 Mo6 O21 101.9(2) . . ? O24 Mo6 O21 99.9(2) . . ? O23 Mo6 O14 98.4(2) . 3_657 ? O24 Mo6 O14 103.3(2) . 3_657 ? O21 Mo6 O14 143.73(18) . 3_657 ? O23 Mo6 O16 161.6(2) . 3_657 ? O24 Mo6 O16 91.9(2) . 3_657 ? O21 Mo6 O16 81.36(16) . 3_657 ? O14 Mo6 O16 70.45(16) 3_657 3_657 ? O23 Mo6 O22 92.0(2) . . ? O24 Mo6 O22 161.8(2) . . ? O21 Mo6 O22 70.17(17) . . ? O14 Mo6 O22 79.49(17) 3_657 . ? O16 Mo6 O22 71.89(14) 3_657 . ? O11 Mn1 O11 180.00(14) 3_756 . ? O11 Mn1 O7 91.77(16) 3_756 . ? O11 Mn1 O7 88.23(16) . . ? O11 Mn1 O7 88.23(16) 3_756 3_756 ? O11 Mn1 O7 91.77(16) . 3_756 ? O7 Mn1 O7 180.000(1) . 3_756 ? O11 Mn1 O12 92.55(16) 3_756 3_756 ? O11 Mn1 O12 87.45(16) . 3_756 ? O7 Mn1 O12 92.93(16) . 3_756 ? O7 Mn1 O12 87.07(16) 3_756 3_756 ? O11 Mn1 O12 87.45(16) 3_756 . ? O11 Mn1 O12 92.55(16) . . ? O7 Mn1 O12 87.07(16) . . ? O7 Mn1 O12 92.93(16) 3_756 . ? O12 Mn1 O12 180.0(2) 3_756 . ? O18 Mn2 O18 180.000(1) 3_657 . ? O18 Mn2 O22 87.17(17) 3_657 3_657 ? O18 Mn2 O22 92.83(17) . 3_657 ? O18 Mn2 O22 92.83(17) 3_657 . ? O18 Mn2 O22 87.17(17) . . ? O22 Mn2 O22 180.000(1) 3_657 . ? O18 Mn2 O16 88.08(17) 3_657 3_657 ? O18 Mn2 O16 91.92(17) . 3_657 ? O22 Mn2 O16 92.14(17) 3_657 3_657 ? O22 Mn2 O16 87.86(17) . 3_657 ? O18 Mn2 O16 91.92(17) 3_657 . ? O18 Mn2 O16 88.08(17) . . ? O22 Mn2 O16 87.86(17) 3_657 . ? O22 Mn2 O16 92.14(17) . . ? O16 Mn2 O16 180.000(1) 3_657 . ? Mo2 O3 Mo1 120.2(2) . . ? Mo3 O6 Mo1 122.9(2) . . ? C4 O7 Mn1 117.1(4) . . ? C4 O7 Mo3 120.5(4) . . ? Mn1 O7 Mo3 100.71(17) . . ? C4 O7 Mo1 123.6(3) . . ? Mn1 O7 Mo1 100.19(16) . . ? Mo3 O7 Mo1 89.24(13) . . ? Mo3 O9 Mo2 122.2(2) . 3_756 ? C2 O11 Mn1 117.9(3) . . ? C2 O11 Mo3 119.3(3) . . ? Mn1 O11 Mo3 100.78(17) . . ? C2 O11 Mo2 123.3(4) . 3_756 ? Mn1 O11 Mo2 100.38(16) . 3_756 ? Mo3 O11 Mo2 89.64(13) . 3_756 ? C3 O12 Mn1 114.7(3) . . ? C3 O12 Mo1 121.1(3) . . ? Mn1 O12 Mo1 101.58(16) . . ? C3 O12 Mo2 121.9(3) . . ? Mn1 O12 Mo2 100.59(15) . . ? Mo1 O12 Mo2 92.65(14) . . ? Mo5 O14 Mo6 120.9(2) . 3_657 ? C12 O16 Mn2 115.4(4) . . ? C12 O16 Mo5 122.5(4) . . ? Mn2 O16 Mo5 99.77(18) . . ? C12 O16 Mo6 122.3(4) . 3_657 ? Mn2 O16 Mo6 99.87(17) . 3_657 ? Mo5 O16 Mo6 91.94(15) . 3_657 ? Mo5 O17 Mo4 121.3(2) . . ? C14 O18 Mn2 117.3(4) . . ? C14 O18 Mo4 121.4(4) . . ? Mn2 O18 Mo4 101.70(17) . . ? C14 O18 Mo5 121.6(4) . . ? Mn2 O18 Mo5 99.95(18) . . ? Mo4 O18 Mo5 89.45(14) . . ? Mo4 O21 Mo6 122.4(2) . . ? C13 O22 Mn2 117.2(4) . . ? C13 O22 Mo4 120.9(4) . . ? Mn2 O22 Mo4 101.06(18) . . ? C13 O22 Mo6 122.1(4) . . ? Mn2 O22 Mo6 100.37(17) . . ? Mo4 O22 Mo6 89.92(15) . . ? C5 N1 C1 128.5(6) . . ? C15 N2 C11 127.3(6) . . ? C33 N3 C25 108.1(5) . . ? C33 N3 C29 111.7(5) . . ? C25 N3 C29 111.1(5) . . ? C33 N3 C21 110.1(5) . . ? C25 N3 C21 110.7(5) . . ? C29 N3 C21 105.3(5) . . ? C45 N4 C49 110.7(5) . . ? C45 N4 C41 112.0(5) . . ? C49 N4 C41 107.6(5) . . ? C45 N4 C37 107.3(5) . . ? C49 N4 C37 109.9(5) . . ? C41 N4 C37 109.4(5) . . ? C53 N5 C61 106.7(8) . . ? C53 N5 C65 110.4(8) . . ? C61 N5 C65 110.9(8) . . ? C53 N5 C57 109.4(9) . . ? C61 N5 C57 113.2(9) . . ? C65 N5 C57 106.2(7) . . ? N1 C1 C4 107.7(5) . 3_756 ? N1 C1 C3 101.9(5) . . ? C4 C1 C3 113.7(5) 3_756 . ? N1 C1 C2 108.6(5) . . ? C4 C1 C2 112.3(5) 3_756 . ? C3 C1 C2 111.8(5) . . ? O11 C2 C1 112.0(5) . . ? O12 C3 C1 113.9(5) . . ? O7 C4 C1 113.2(5) . 3_756 ? O25 C5 N1 124.6(6) . . ? O25 C5 C6 122.4(7) . . ? N1 C5 C6 112.9(6) . . ? C7 C6 C5 112.4(6) . . ? C9 C7 C6 109.8(7) . . ? C9 C7 C8 109.2(7) . . ? C6 C7 C8 112.7(6) . . ? C9 C7 C10 110.4(7) . . ? C6 C7 C10 107.2(7) . . ? C8 C7 C10 107.4(6) . . ? O26 C8 O27 123.8(8) . . ? O26 C8 C7 124.6(7) . . ? O27 C8 C7 111.4(7) . . ? N2 C11 C14 103.4(5) . 3_657 ? N2 C11 C12 108.5(5) . . ? C14 C11 C12 112.2(5) 3_657 . ? N2 C11 C13 107.1(5) . . ? C14 C11 C13 111.7(6) 3_657 . ? C12 C11 C13 113.2(6) . . ? O16 C12 C11 113.0(5) . . ? O22 C13 C11 113.5(5) . . ? O18 C14 C11 113.7(5) . 3_657 ? O28 C15 N2 123.4(7) . . ? O28 C15 C16 120.6(7) . . ? N2 C15 C16 116.0(7) . . ? C17 C16 C15 112.5(6) . . ? C18 C17 C16 113.2(6) . . ? C18 C17 C19 108.6(6) . . ? C16 C17 C19 107.7(7) . . ? C18 C17 C20 108.8(7) . . ? C16 C17 C20 108.3(6) . . ? C19 C17 C20 110.2(7) . . ? O30 C18 O29 122.6(7) . . ? O30 C18 C17 125.6(8) . . ? O29 C18 C17 111.6(7) . . ? C22 C21 N3 115.8(5) . . ? C21 C22 C23 110.9(6) . . ? C24 C23 C22 113.3(6) . . ? C26 C25 N3 115.3(6) . . ? C27 C26 C25 112.8(7) . . ? C26 C27 C28 113.0(8) . . ? C30 C29 N3 116.3(5) . . ? C29 C30 C31 110.1(6) . . ? C32 C31 C30 114.0(6) . . ? N3 C33 C34 115.5(6) . . ? C35 C34 C33 110.8(7) . . ? C36 C35 C34 110.7(9) . . ? C38 C37 N4 114.9(6) . . ? C39 C38 C37 111.8(6) . . ? C38 C39 C40 112.4(7) . . ? C42 C41 N4 115.5(6) . . ? C41 C42 C43 111.0(6) . . ? C44 C43 C42 115.1(7) . . ? N4 C45 C46 114.1(6) . . ? C47 C46 C45 112.9(6) . . ? C46 C47 C48 111.8(7) . . ? N4 C49 C50 115.9(5) . . ? C51 C50 C49 111.6(6) . . ? C50 C51 C52 112.7(7) . . ? N5 C53 C54 116.0(9) . . ? C53 C54 C55 110.4(9) . . ? C56 C55 C54 112.2(10) . . ? N5 C57 C58 113.9(8) . . ? C57 C58 C59 108.4(9) . . ? C60 C59 C58 108.1(12) . . ? C62 C61 N5 115.9(9) . . ? C61 C62 C63 111.2(10) . . ? C64 C63 C62 113.4(11) . . ? N5 C65 C66 114.4(8) . . ? C67 C66 C65 111.2(9) . . ? C66 C67 C68 102.5(14) . . ? N6 C69 C70 172.9(19) . . ? N7 C71 C72 176.6(13) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O27 H27 O15 0.84 1.81 2.639(7) 172.0 1_654 O29 H29 O10 0.84 1.95 2.783(6) 173.6 4_566 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.83 _refine_diff_density_min -0.91 _refine_diff_density_rms 0.13 data_mh1172 _database_code_depnum_ccdc_archive 'CCDC 909169' #TrackingRef 'MnMo6-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H146 Mn Mo6 N7 O32' _chemical_formula_weight 2324.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pmna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x, -y, -z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x, y, z' 'x-1/2, -y, z-1/2' _cell_length_a 23.8498(6) _cell_length_b 14.5730(3) _cell_length_c 15.4775(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5379.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15240 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 25.9 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 0.862 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.80 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Oxford Gemini Ultra CCD' _diffrn_measurement_method '\w & \p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 43374 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5414 _reflns_number_gt 4383 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics diamond3 _computing_publication_material WinGX _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^ > 2\s(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^)+(0.1180P)^2^+29.3874P] 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 none _refine_ls_number_reflns 5414 _refine_ls_number_parameters 249 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.2248 _refine_ls_wR_factor_gt 0.2065 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.006 _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 0.35936(3) 0.0000 0.5000 0.0417(3) Uani 1 2 d S . . Mo2 Mo 0.42970(2) 0.16189(3) 0.38984(3) 0.0335(2) Uani 1 1 d . . . Mn1 Mn 0.5000 0.0000 0.5000 0.0187(3) Uani 1 4 d S . . O1 O 0.4282(2) 0.1803(4) 0.2817(3) 0.0516(13) Uani 1 1 d . . . O2 O 0.5000 0.2143(4) 0.4241(4) 0.0324(12) Uani 1 2 d S . . O3 O 0.5000 0.0503(4) 0.3777(3) 0.0303(12) Uani 1 2 d S . . O4 O 0.38380(18) 0.0534(3) 0.3929(3) 0.0399(10) Uani 1 1 d . . . O5 O 0.3862(2) 0.2422(3) 0.4330(3) 0.0480(11) Uani 1 1 d . . . O6 O 0.3163(2) 0.0828(4) 0.5396(4) 0.0637(15) Uani 1 1 d . . . O7 O 0.44060(16) 0.0885(3) 0.5264(2) 0.0276(8) Uani 1 1 d . . . O8 O 0.5154(5) 0.3147(6) 0.6800(6) 0.059(5) Uani 0.50 1 d P . . O9 O 0.5999(8) 0.2756(13) 0.8232(12) 0.112(5) Uiso 0.50 1 d PD . 1 O10 O 0.6000(15) 0.329(2) 0.954(2) 0.099(9) Uiso 0.25 1 d PD . 1 O10' O 0.611(2) 0.389(3) 0.895(3) 0.115(14) Uiso 0.25 1 d P . 2 O11 O 0.5246(6) 0.0902(10) 0.8981(9) 0.085(4) Uiso 0.50 1 d P . . C1 C 0.5000 -0.0165(6) 0.3095(5) 0.0365(19) Uani 1 2 d S . . H1A H 0.5335 -0.0070 0.2729 0.044 Uiso 0.50 1 calc PR . . H1B H 0.4665 -0.0070 0.2729 0.044 Uiso 0.50 1 calc PR . . C2 C 0.5000 0.1174(5) 0.6561(5) 0.0330(17) Uani 1 2 d S . . C3 C 0.4464(3) 0.1402(4) 0.6053(4) 0.0355(13) Uani 1 1 d . . . H3A H 0.4135 0.1280 0.6425 0.043 Uiso 1 1 calc R . . H3B H 0.4465 0.2065 0.5911 0.043 Uiso 1 1 calc R . . C4 C 0.5000 0.2648(7) 0.7410(7) 0.056(3) Uani 1 2 d S . . C5 C 0.4819(5) 0.3075(8) 0.8261(7) 0.054(4) Uiso 0.50 1 d PG . . C6 C 0.4249(4) 0.3254(12) 0.8351(11) 0.092(7) Uiso 0.50 1 d PG . . C7 C 0.4051(6) 0.3695(16) 0.9086(14) 0.17(2) Uiso 0.50 1 d PG . . C8 C 0.4423(9) 0.3957(13) 0.9732(10) 0.116(9) Uiso 0.50 1 d PG . . C9 C 0.4998(8) 0.3779(9) 0.9643(7) 0.096(5) Uiso 1 2 d SG . . C10 C 0.5190(4) 0.3338(8) 0.8907(8) 0.065(5) Uiso 0.50 1 d PG . . C11 C 0.5745(13) 0.314(2) 0.8830(17) 0.114(10) Uiso 0.50 1 d PD . 1 C24 C 0.5000 0.1133(13) 0.9496(11) 0.104(5) Uiso 1 2 d SD . . C14 C 0.2416(8) 0.1787(12) 0.1664(10) 0.087(5) Uiso 0.60 1 d PD A 1 C14' C 0.2995(12) 0.2792(19) 0.2705(19) 0.103(9) Uiso 0.40 1 d PD B 2 C15 C 0.3014(8) 0.0709(14) 0.2311(13) 0.070(5) Uiso 0.50 1 d P C 1 C16 C 0.2943(10) 0.0088(16) 0.1530(16) 0.079(6) Uiso 0.50 1 d P C 1 C17 C 0.3367(13) -0.076(2) 0.159(2) 0.094(8) Uiso 0.40 1 d P C 1 C15' C 0.3090(14) 0.100(2) 0.192(2) 0.072(8) Uiso 0.30 1 d P D 2 C16' C 0.3059(17) 0.042(3) 0.120(3) 0.086(10) Uiso 0.30 1 d P D 2 C17' C 0.3509(16) -0.030(3) 0.130(2) 0.078(9) Uiso 0.30 1 d P D 2 C18 C 0.2817(12) 0.2513(19) 0.137(2) 0.112(10) Uiso 0.40 1 d PD A 1 C18' C 0.3158(15) 0.352(2) 0.206(2) 0.085(10) Uiso 0.30 1 d PD B 2 C19 C 0.2586(19) 0.325(3) 0.077(3) 0.106(13) Uiso 0.30 1 d PD . 1 C19' C 0.3708(16) 0.399(3) 0.228(3) 0.132(17) Uiso 0.30 1 d PD B 2 C20' C 0.4301(19) 0.401(5) 0.201(4) 0.11(2) Uiso 0.20 1 d PD B 2 C20 C 0.223(2) 0.713(4) 0.464(3) 0.087(15) Uiso 0.20 1 d PD . 1 C21 C 0.3264(11) 0.7037(19) 0.3629(18) 0.105(7) Uiso 0.50 1 d PD . 1 C22 C 0.2319(18) 0.619(3) 0.349(3) 0.102(12) Uiso 0.30 1 d PD . 1 C23 C 0.4609(15) 0.161(3) 1.1061(19) 0.148(14) Uiso 0.50 1 d PD . 1 C23' C 0.4376(9) 0.142(3) 1.058(3) 0.139(15) Uiso 0.40 1 d PD . 2 C25 C 0.4454(16) 0.529(2) 0.452(2) 0.116(11) Uiso 0.40 1 d PD . 1 C25' C 0.4744(18) 0.5000 0.5000 0.100(13) Uiso 0.40 2 d SP . 2 C26 C 0.465(2) 0.439(3) 0.412(3) 0.097(17) Uiso 0.20 1 d PD . 1 C27 C 0.5000 0.447(3) 0.332(3) 0.119(13) Uiso 0.50 2 d SPD . 1 N1 N 0.5000 0.1740(5) 0.7351(5) 0.046(2) Uani 1 2 d S . . H1 H 0.5000 0.1438 0.7844 0.055 Uiso 1 2 calc SR . . N2 N 0.2500 0.1312(13) 0.2500 0.074(5) Uiso 0.60 2 d SPD . 1 N2' N 0.2500 0.219(2) 0.2500 0.096(10) Uiso 0.40 2 d SPD . 2 N3 N 0.2665(16) 0.690(4) 0.395(4) 0.12(2) Uiso 0.15 1 d PD . . N4 N 0.5000 0.1386(10) 1.0366(9) 0.092(4) Uiso 1 2 d SD . . 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 0.0213(4) 0.0458(5) 0.0580(6) 0.0051(4) 0.000 0.000 Mo2 0.0365(4) 0.0327(3) 0.0313(3) 0.0029(2) -0.00878(19) 0.00451(19) Mn1 0.0185(7) 0.0229(7) 0.0147(7) -0.0009(5) 0.000 0.000 O1 0.067(4) 0.051(3) 0.036(3) 0.008(2) -0.013(2) 0.002(2) O2 0.040(3) 0.031(3) 0.027(3) -0.001(2) 0.000 0.000 O3 0.035(3) 0.030(3) 0.026(3) -0.006(2) 0.000 0.000 O4 0.035(2) 0.042(2) 0.043(2) 0.0004(19) -0.0134(18) -0.0006(18) O5 0.045(3) 0.045(2) 0.055(3) 0.000(2) -0.005(2) 0.013(2) O6 0.035(3) 0.058(3) 0.098(4) 0.004(3) 0.016(3) 0.015(2) O7 0.0281(19) 0.0319(19) 0.0229(18) -0.0013(15) 0.0005(14) -0.0003(16) O8 0.100(16) 0.038(4) 0.039(5) -0.005(4) 0.010(5) -0.004(5) C1 0.049(5) 0.036(4) 0.024(4) -0.008(3) 0.000 0.000 C2 0.045(5) 0.031(4) 0.023(4) -0.006(3) 0.000 0.000 C3 0.041(3) 0.036(3) 0.030(3) -0.007(2) 0.009(2) 0.006(3) C4 0.098(9) 0.033(5) 0.038(5) -0.010(4) 0.000 0.000 N1 0.083(6) 0.035(4) 0.020(4) -0.004(3) 0.000 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O6 1.699(5) . ? Mo1 O6 1.699(5) 3_556 ? Mo1 O4 1.922(4) 3_556 ? Mo1 O4 1.922(4) . ? Mo1 O7 2.364(4) . ? Mo1 O7 2.364(4) 3_556 ? Mo2 O1 1.696(5) . ? Mo2 O5 1.700(5) . ? Mo2 O2 1.917(3) . ? Mo2 O4 1.924(4) . ? Mo2 O3 2.344(4) . ? Mo2 O7 2.383(4) . ? Mn1 O7 1.959(4) 7_655 ? Mn1 O7 1.959(4) 3_556 ? Mn1 O7 1.959(4) . ? Mn1 O7 1.959(4) 5_656 ? Mn1 O3 2.029(5) . ? Mn1 O3 2.029(5) 5_656 ? O2 Mo2 1.917(3) 7_655 ? O3 C1 1.436(9) . ? O3 Mo2 2.344(4) 7_655 ? O7 C3 1.441(7) . ? O8 O8 0.74(3) 7_655 ? O8 C4 1.247(13) . ? O9 C6 0.95(3) 7_655 ? O9 C11 1.24(2) . ? O9 C7 1.91(3) 7_655 ? O10 C7 0.93(5) 7_655 ? O10 C11 1.27(3) . ? O10 C8 1.44(4) 7_655 ? O10' C7 0.52(6) 7_655 ? O10' C6 1.57(5) 7_655 ? O10' C8 1.75(5) 7_655 ? O11 C24 1.045(16) . ? O11 O11 1.17(3) 7_655 ? C1 C2 1.564(11) 5_656 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N1 1.475(10) . ? C2 C3 1.537(8) . ? C2 C3 1.537(8) 7_655 ? C2 C1 1.564(11) 5_656 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O8 1.247(13) 7_655 ? C4 N1 1.326(12) . ? C4 C5 1.521(13) 7_655 ? C4 C5 1.521(13) . ? C5 C5 0.86(2) 7_655 ? C5 C10 1.0709 7_655 ? C5 C6 1.3900 . ? C5 C10 1.3900 . ? C5 C11 1.61(3) 7_655 ? C6 C11 0.76(3) 7_655 ? C6 O9 0.95(2) 7_655 ? C6 C7 1.3900 . ? C6 O10' 1.57(5) 7_655 ? C6 C10 1.595(18) 7_655 ? C7 O10' 0.52(6) 7_655 ? C7 O10 0.93(4) 7_655 ? C7 C11 1.03(4) 7_655 ? C7 C8 1.3900 . ? C7 C10 1.90(2) 7_655 ? C7 O9 1.91(3) 7_655 ? C8 C9 1.4038 . ? C8 O10 1.44(4) 7_655 ? C8 O10' 1.75(5) 7_655 ? C8 C10 1.816(11) 7_655 ? C8 C11 1.88(3) 7_655 ? C9 C10 1.383(7) 7_655 ? C9 C10 1.3853 . ? C9 C8 1.41(4) 7_655 ? C10 C10 0.91(2) 7_655 ? C10 C5 1.071(8) 7_655 ? C10 C11 1.36(3) . ? C10 C6 1.595(17) 7_655 ? C10 C8 1.82(2) 7_655 ? C10 C7 1.90(3) 7_655 ? C11 C6 0.76(4) 7_655 ? C11 C7 1.03(4) 7_655 ? C11 C5 1.61(3) 7_655 ? C11 C8 1.88(3) 7_655 ? C24 O11 1.045(16) 7_655 ? C24 N4 1.396(15) . ? C14 N2 1.481(15) . ? C14 C18 1.499(18) . ? C14' C18' 1.504(19) . ? C14' N2' 1.504(18) . ? C15 C16 1.52(3) . ? C15 N2 1.54(2) . ? C16 C17 1.60(4) . ? C15' C16' 1.40(5) . ? C16' C17' 1.51(5) . ? C18 C19 1.525(19) . ? C18' C19' 1.518(19) . ? C19 C20 1.90(7) 2_564 ? C19' C20' 1.47(2) . ? C20 N3 1.53(2) . ? C20 C19 1.90(7) 2_565 ? C21 N3 1.523(19) . ? C22 N3 1.50(2) . ? C23 N4 1.460(18) . ? C23 C23 1.87(7) 7_655 ? C23' N4 1.523(19) . ? C25 C26 1.53(2) . ? C25 C25 1.70(8) 3_566 ? C25' C25' 1.22(9) 5_666 ? C26 C27 1.49(2) . ? C26 C26 1.67(11) 7_655 ? C27 C26 1.49(2) 7_655 ? N1 H1 0.8800 . ? N2 C14 1.481(15) 4 ? N2 C15 1.54(2) 4 ? N2' C14' 1.504(18) 4 ? N4 C23 1.460(18) 7_655 ? N4 C23' 1.523(19) 7_655 ? 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 O6 Mo1 O6 105.6(4) . 3_556 ? O6 Mo1 O4 99.2(2) . 3_556 ? O6 Mo1 O4 102.0(2) 3_556 3_556 ? O6 Mo1 O4 102.0(2) . . ? O6 Mo1 O4 99.2(2) 3_556 . ? O4 Mo1 O4 144.7(2) 3_556 . ? O6 Mo1 O7 92.6(2) . . ? O6 Mo1 O7 161.0(2) 3_556 . ? O4 Mo1 O7 79.80(16) 3_556 . ? O4 Mo1 O7 71.32(15) . . ? O6 Mo1 O7 161.0(2) . 3_556 ? O6 Mo1 O7 92.6(2) 3_556 3_556 ? O4 Mo1 O7 71.32(15) 3_556 3_556 ? O4 Mo1 O7 79.80(16) . 3_556 ? O7 Mo1 O7 69.88(18) . 3_556 ? O1 Mo2 O5 105.4(2) . . ? O1 Mo2 O2 103.2(2) . . ? O5 Mo2 O2 98.7(2) . . ? O1 Mo2 O4 98.2(2) . . ? O5 Mo2 O4 102.1(2) . . ? O2 Mo2 O4 144.9(2) . . ? O1 Mo2 O3 92.6(2) . . ? O5 Mo2 O3 161.0(2) . . ? O2 Mo2 O3 70.90(17) . . ? O4 Mo2 O3 80.70(17) . . ? O1 Mo2 O7 161.6(2) . . ? O5 Mo2 O7 91.51(19) . . ? O2 Mo2 O7 80.68(19) . . ? O4 Mo2 O7 70.83(15) . . ? O3 Mo2 O7 71.44(16) . . ? O7 Mn1 O7 180.0(2) 7_655 3_556 ? O7 Mn1 O7 92.6(2) 7_655 . ? O7 Mn1 O7 87.4(2) 3_556 . ? O7 Mn1 O7 87.4(2) 7_655 5_656 ? O7 Mn1 O7 92.6(2) 3_556 5_656 ? O7 Mn1 O7 180.0(2) . 5_656 ? O7 Mn1 O3 87.54(15) 7_655 . ? O7 Mn1 O3 92.46(15) 3_556 . ? O7 Mn1 O3 87.54(15) . . ? O7 Mn1 O3 92.46(15) 5_656 . ? O7 Mn1 O3 92.46(15) 7_655 5_656 ? O7 Mn1 O3 87.54(15) 3_556 5_656 ? O7 Mn1 O3 92.46(15) . 5_656 ? O7 Mn1 O3 87.54(15) 5_656 5_656 ? O3 Mn1 O3 180.000(1) . 5_656 ? Mo2 O2 Mo2 122.0(3) . 7_655 ? C1 O3 Mn1 116.2(5) . . ? C1 O3 Mo2 122.0(3) . 7_655 ? Mn1 O3 Mo2 100.13(17) . 7_655 ? C1 O3 Mo2 122.0(3) . . ? Mn1 O3 Mo2 100.13(17) . . ? Mo2 O3 Mo2 91.34(19) 7_655 . ? Mo1 O4 Mo2 121.8(2) . . ? C3 O7 Mn1 116.8(3) . . ? C3 O7 Mo1 120.7(3) . . ? Mn1 O7 Mo1 101.37(16) . . ? C3 O7 Mo2 121.8(3) . . ? Mn1 O7 Mo2 100.89(15) . . ? Mo1 O7 Mo2 90.11(13) . . ? O8 O8 C4 72.8(6) 7_655 . ? C6 O9 C11 38(2) 7_655 . ? C6 O9 C7 44.1(11) 7_655 7_655 ? C11 O9 C7 29.4(17) . 7_655 ? C7 O10 C11 53(3) 7_655 . ? C7 O10 C8 68(2) 7_655 7_655 ? C11 O10 C8 88(3) . 7_655 ? C7 O10' C6 61(5) 7_655 7_655 ? C7 O10' C8 39(4) 7_655 7_655 ? C6 O10' C8 93(3) 7_655 7_655 ? C24 O11 O11 55.9(9) . 7_655 ? O3 C1 C2 112.8(7) . 5_656 ? O3 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 5_656 . ? O3 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 5_656 . ? H1A C1 H1B 107.8 . . ? N1 C2 C3 107.7(4) . . ? N1 C2 C3 107.7(4) . 7_655 ? C3 C2 C3 112.5(7) . 7_655 ? N1 C2 C1 104.1(6) . 5_656 ? C3 C2 C1 112.2(4) . 5_656 ? C3 C2 C1 112.2(4) 7_655 5_656 ? O7 C3 C2 113.6(5) . . ? O7 C3 H3A 108.8 . . ? C2 C3 H3A 108.8 . . ? O7 C3 H3B 108.8 . . ? C2 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? O8 C4 O8 34.3(12) 7_655 . ? O8 C4 N1 122.1(9) 7_655 . ? O8 C4 N1 122.1(9) . . ? O8 C4 C5 120.0(9) 7_655 7_655 ? O8 C4 C5 109.4(8) . 7_655 ? N1 C4 C5 117.9(9) . 7_655 ? O8 C4 C5 109.4(8) 7_655 . ? O8 C4 C5 120.0(9) . . ? N1 C4 C5 117.9(9) . . ? C5 C4 C5 33.0(9) 7_655 . ? C5 C5 C10 91.2(10) 7_655 7_655 ? C5 C5 C6 167.8(6) 7_655 . ? C10 C5 C6 79.6(11) 7_655 . ? C5 C5 C10 50.4(5) 7_655 . ? C10 C5 C10 40.8(11) 7_655 . ? C6 C5 C10 120.0 . . ? C5 C5 C4 73.5(4) 7_655 . ? C10 C5 C4 164.0(14) 7_655 . ? C6 C5 C4 116.2(8) . . ? C10 C5 C4 123.7(8) . . ? C5 C5 C11 146.6(10) 7_655 7_655 ? C10 C5 C11 56.8(12) 7_655 7_655 ? C6 C5 C11 28.2(12) . 7_655 ? C10 C5 C11 97.1(11) . 7_655 ? C4 C5 C11 137.3(13) . 7_655 ? C11 C6 O9 92(3) 7_655 7_655 ? C11 C6 C7 46(3) 7_655 . ? O9 C6 C7 107.4(18) 7_655 . ? C11 C6 C5 92(3) 7_655 . ? O9 C6 C5 116.4(18) 7_655 . ? C7 C6 C5 120.0 . . ? C11 C6 O10' 64(3) 7_655 7_655 ? O9 C6 O10' 103(2) 7_655 7_655 ? C7 C6 O10' 19(2) . 7_655 ? C5 C6 O10' 134.7(19) . 7_655 ? C11 C6 C10 58(2) 7_655 7_655 ? O9 C6 C10 133.1(18) 7_655 7_655 ? C7 C6 C10 78.9(4) . 7_655 ? C5 C6 C10 41.3(4) . 7_655 ? O10' C6 C10 95.2(19) 7_655 7_655 ? O10' C7 O10 123(6) 7_655 7_655 ? O10' C7 C11 129(6) 7_655 7_655 ? O10 C7 C11 81(3) 7_655 7_655 ? O10' C7 C6 100(5) 7_655 . ? O10 C7 C6 111(2) 7_655 . ? C11 C7 C6 32.6(19) 7_655 . ? O10' C7 C8 128(6) 7_655 . ? O10 C7 C8 74(3) 7_655 . ? C11 C7 C8 101.2(18) 7_655 . ? C6 C7 C8 120.0 . . ? O10' C7 C10 143(6) 7_655 7_655 ? O10 C7 C10 93(2) 7_655 7_655 ? C11 C7 C10 43.7(19) 7_655 7_655 ? C6 C7 C10 55.35(16) . 7_655 ? C8 C7 C10 64.77(16) . 7_655 ? O10' C7 O9 94(5) 7_655 7_655 ? O10 C7 O9 93(3) 7_655 7_655 ? C11 C7 O9 36.3(18) 7_655 7_655 ? C6 C7 O9 28.5(8) . 7_655 ? C8 C7 O9 137.5(8) . 7_655 ? C10 C7 O9 76.3(7) 7_655 7_655 ? C9 C8 C7 120.1 . . ? C9 C8 O10 122.6(16) . 7_655 ? C7 C8 O10 38.2(16) . 7_655 ? C9 C8 O10' 129.0(15) . 7_655 ? C7 C8 O10' 13.5(17) . 7_655 ? O10 C8 O10' 46(2) 7_655 7_655 ? C9 C8 C10 48.8(6) . 7_655 ? C7 C8 C10 71.4(6) . 7_655 ? O10 C8 C10 82.6(15) 7_655 7_655 ? O10' C8 C10 81.7(16) 7_655 7_655 ? C9 C8 C11 91.0(10) . 7_655 ? C7 C8 C11 32.4(11) . 7_655 ? O10 C8 C11 42.5(15) 7_655 7_655 ? O10' C8 C11 45.4(18) 7_655 7_655 ? C10 C8 C11 43.1(9) 7_655 7_655 ? C10 C9 C8 81.3(8) 7_655 . ? C10 C9 C10 38.3(8) 7_655 . ? C8 C9 C10 119.4 . . ? C10 C9 C8 119.0(11) 7_655 7_655 ? C8 C9 C8 155.8(4) . 7_655 ? C10 C9 C8 81.0(3) . 7_655 ? C10 C10 C5 88.8(12) 7_655 7_655 ? C10 C10 C11 166.6(15) 7_655 . ? C5 C10 C11 82.0(15) 7_655 . ? C10 C10 C9 70.7 7_655 . ? C5 C10 C9 157.9(11) 7_655 . ? C11 C10 C9 119.5(14) . . ? C10 C10 C5 50.4 7_655 . ? C5 C10 C5 38.5(12) 7_655 . ? C11 C10 C5 119.9(14) . . ? C9 C10 C5 120.5 . . ? C10 C10 C6 146.9(4) 7_655 7_655 ? C5 C10 C6 59.0(8) 7_655 7_655 ? C11 C10 C6 28.5(16) . 7_655 ? C9 C10 C6 139.2(3) . 7_655 ? C5 C10 C6 97.2(4) . 7_655 ? C10 C10 C8 120.5(11) 7_655 7_655 ? C5 C10 C8 147.6(14) 7_655 7_655 ? C11 C10 C8 71.0(13) . 7_655 ? C9 C10 C8 50.1(11) . 7_655 ? C5 C10 C8 165.2(8) . 7_655 ? C6 C10 C8 89.6(12) 7_655 7_655 ? C10 C10 C7 162.0(2) 7_655 7_655 ? C5 C10 C7 104.7(12) 7_655 7_655 ? C11 C10 C7 31.4(15) . 7_655 ? C9 C10 C7 93.9(2) . 7_655 ? C5 C10 C7 141.86(14) . 7_655 ? C6 C10 C7 45.8(5) 7_655 7_655 ? C8 C10 C7 43.8(9) 7_655 7_655 ? C6 C11 C7 101(4) 7_655 7_655 ? C6 C11 O9 50(2) 7_655 . ? C7 C11 O9 114(3) 7_655 . ? C6 C11 O10 142(4) 7_655 . ? C7 C11 O10 46(3) 7_655 . ? O9 C11 O10 119(3) . . ? C6 C11 C10 93(3) 7_655 . ? C7 C11 C10 105(3) 7_655 . ? O9 C11 C10 130(2) . . ? O10 C11 C10 111(3) . . ? C6 C11 C5 60(2) 7_655 7_655 ? C7 C11 C5 131(3) 7_655 7_655 ? O9 C11 C5 88.5(18) . 7_655 ? O10 C11 C5 152(3) . 7_655 ? C10 C11 C5 41.2(9) . 7_655 ? C6 C11 C8 126(4) 7_655 7_655 ? C7 C11 C8 46.5(16) 7_655 7_655 ? O9 C11 C8 161(3) . 7_655 ? O10 C11 C8 50(2) . 7_655 ? C10 C11 C8 65.9(13) . 7_655 ? C5 C11 C8 105.3(19) 7_655 7_655 ? O11 C24 O11 68.2(19) 7_655 . ? O11 C24 N4 145.2(10) 7_655 . ? O11 C24 N4 145.2(10) . . ? N2 C14 C18 120.8(19) . . ? C18' C14' N2' 118(2) . . ? C16 C15 N2 113.8(16) . . ? C15 C16 C17 110(2) . . ? C15' C16' C17' 107(3) . . ? C14 C18 C19 117(3) . . ? C14' C18' C19' 113(3) . . ? C18 C19 C20 105(3) . 2_564 ? C20' C19' C18' 141(5) . . ? N3 C20 C19 115(4) . 2_565 ? N4 C23 C23 50.3(17) . 7_655 ? C26 C25 C25 86(3) . 3_566 ? C27 C26 C25 116(4) . . ? C27 C26 C26 56(2) . 7_655 ? C25 C26 C26 108(3) . 7_655 ? C26 C27 C26 68(5) 7_655 . ? C4 N1 C2 127.8(8) . . ? C4 N1 H1 116.1 . . ? C2 N1 H1 116.1 . . ? C14 N2 C14 124.3(19) 4 . ? C14 N2 C15 109.0(10) 4 . ? C14 N2 C15 102.1(11) . . ? C14 N2 C15 102.1(11) 4 4 ? C14 N2 C15 109.0(11) . 4 ? C15 N2 C15 110(2) . 4 ? C14' N2' C14' 109(3) . 4 ? C22 N3 C21 117(3) . . ? C22 N3 C20 96(3) . . ? C21 N3 C20 147(4) . . ? C24 N4 C23 140.3(17) . 7_655 ? C24 N4 C23 140.3(17) . . ? C23 N4 C23 79(3) 7_655 . ? C24 N4 C23' 102(2) . 7_655 ? C23 N4 C23' 38(2) 7_655 7_655 ? C23 N4 C23' 117(3) . 7_655 ? C24 N4 C23' 102(2) . . ? C23 N4 C23' 117(3) 7_655 . ? C23 N4 C23' 38(2) . . ? C23' N4 C23' 155(4) 7_655 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.11 _refine_diff_density_min -1.01 _refine_diff_density_rms 0.16 data_mh248 _database_code_depnum_ccdc_archive 'CCDC 909170' #TrackingRef 'MnMo6-8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C143 H219 Mn Mo6 N10 O37' _chemical_formula_weight 3300.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 23.5808(3) _cell_length_b 24.7645(3) _cell_length_c 29.9716(4) _cell_angle_alpha 100.967(2) _cell_angle_beta 103.918(2) _cell_angle_gamma 93.897(2) _cell_volume 16559.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 36757 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 26.0 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6880 _exptl_absorpt_coefficient_mu 0.585 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7169 _exptl_absorpt_correction_T_max 0.8488 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Oxford Gemini Ultra A CCD' _diffrn_measurement_method '\w & \p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 262887 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 26.00 _reflns_number_total 64939 _reflns_number_gt 26110 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics diamond3 _computing_publication_material WinGX _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^ > 2\s(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^)+(0.0918P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 64939 _refine_ls_number_parameters 3214 _refine_ls_number_restraints 1248 _refine_ls_R_factor_all 0.1114 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1866 _refine_ls_wR_factor_gt 0.1622 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.003452(8) 0.865659(8) 0.004970(7) 0.02260(5) Uani 1 1 d . G . Mo2 Mo -0.070965(9) 0.900892(8) -0.093956(7) 0.02401(6) Uani 1 1 d . G . Mo3 Mo 0.074443(8) 0.964553(8) 0.098736(6) 0.02251(5) Uani 1 1 d . . . Mo4 Mo 0.574494(8) 0.464505(8) 0.098738(7) 0.02223(6) Uani 1 1 d . H . Mo5 Mo 0.571019(9) 0.599183(8) 0.093980(7) 0.02375(6) Uani 1 1 d . H . Mo6 Mo 0.503406(9) 0.365589(8) 0.004911(7) 0.02310(6) Uani 1 1 d . . . Mo7 Mo 0.738111(8) 0.881452(8) 0.485964(7) 0.02149(5) Uani 1 1 d . . . Mo8 Mo 0.672051(8) 0.773599(8) 0.397863(6) 0.02156(5) Uani 1 1 d . . . Mo9 Mo 0.680452(8) 0.643514(8) 0.413459(6) 0.02131(5) Uani 1 1 d . . . Mo10 Mo 0.761845(8) 0.618550(8) 0.514023(7) 0.02150(6) Uani 1 1 d . . . Mo11 Mo 0.827990(8) 0.726351(8) 0.602120(7) 0.02186(6) Uani 1 1 d . . . Mo12 Mo 0.819482(8) 0.856440(8) 0.586546(7) 0.02115(6) Uani 1 1 d . . . Mn1 Mn 0.0000 1.0000 0.0000 0.01680(12) Uani 1 2 d S . . Mn2 Mn 0.5000 0.5000 0.0000 0.01442(12) Uani 1 2 d S . . Mn3 Mn 0.750089(19) 0.750075(19) 0.500082(15) 0.01503(6) Uani 1 1 d . . . O1 O -0.02358(7) 0.83058(6) 0.04112(5) 0.0317(5) Uani 1 1 d . . . O2 O 0.03481(7) 0.81808(6) -0.02827(5) 0.0347(5) Uani 1 1 d . . . O3 O -0.01695(6) 0.95102(6) 0.04293(5) 0.0215(4) Uani 1 1 d . . . O4 O -0.06881(6) 0.87128(6) -0.03853(5) 0.0253(4) Uani 1 1 d . . . O5 O 0.02092(6) 0.93361(6) -0.03853(4) 0.0203(4) Uani 1 1 d . . . O6 O -0.14468(7) 0.89009(7) -0.11896(5) 0.0381(5) Uani 1 1 d . . . O7 O -0.07950(6) 0.98218(6) -0.04067(5) 0.0203(4) Uani 1 1 d . . . O8 O -0.04856(6) 0.96467(6) -0.11703(5) 0.0251(4) Uani 1 1 d . . . O9 O 0.07520(6) 0.90557(6) 0.04705(5) 0.0225(4) Uani 1 1 d . . . O10 O 0.14877(7) 0.97780(7) 0.12331(6) 0.0368(5) Uani 1 1 d . . . O11 O 0.04782(7) 0.93059(6) 0.13478(5) 0.0338(5) Uani 1 1 d . . . O12 O -0.04053(7) 0.85213(6) -0.12660(6) 0.0386(5) Uani 1 1 d . . . O13 O -0.22258(7) 1.04467(7) 0.01043(6) 0.0401(5) Uani 1 1 d . . . O14 O -0.19923(7) 1.11707(7) 0.11035(6) 0.0434(6) Uani 1 1 d . . . H14A H -0.1885 1.1490 0.1075 0.065 Uiso 1 1 calc R A 1 O15 O -0.28996(6) 1.13601(7) 0.07904(6) 0.0453(6) Uani 1 1 d . . . O16 O 0.54880(6) 0.53596(6) 0.11687(5) 0.0266(5) Uani 1 1 d . . . O17 O 0.64485(7) 0.61000(7) 0.11854(6) 0.0369(5) Uani 1 1 d . . . O18 O 0.57953(6) 0.51784(6) 0.04109(5) 0.0223(4) Uani 1 1 d . . . O19 O 0.54099(7) 0.64772(7) 0.12704(5) 0.0363(5) Uani 1 1 d . . . O20 O 0.47896(6) 0.56682(6) 0.03883(5) 0.0230(4) Uani 1 1 d . . . O21 O 0.56865(6) 0.62835(6) 0.03877(5) 0.0242(5) Uani 1 1 d . . . O22 O 0.48283(6) 0.45123(6) 0.04286(5) 0.0215(4) Uani 1 1 d . . . O23 O 0.53497(7) 0.31847(6) -0.02805(5) 0.0330(5) Uani 1 1 d . . . O24 O 0.47712(7) 0.33055(6) 0.04097(5) 0.0309(5) Uani 1 1 d . . . O25 O 0.57475(6) 0.40600(6) 0.04677(5) 0.0247(5) Uani 1 1 d . . . O26 O 0.64806(7) 0.47841(7) 0.12306(6) 0.0389(6) Uani 1 1 d . . . O27 O 0.54711(7) 0.42999(6) 0.13484(5) 0.0316(5) Uani 1 1 d . . . O28 O 0.72144(7) 0.45531(7) -0.00999(6) 0.0442(6) Uani 1 1 d . . . O29 O 0.69867(7) 0.38362(7) -0.11001(7) 0.0467(6) Uani 1 1 d . . . H29B H 0.6905 0.3490 -0.1173 0.070 Uiso 1 1 calc R B 1 O30 O 0.78920(8) 0.36397(6) -0.07985(7) 0.0488(6) Uani 1 1 d . . . O31 O 0.70044(6) 0.70290(6) 0.38520(5) 0.0236(4) Uani 1 1 d . . . O32 O 0.60538(6) 0.63521(6) 0.39402(5) 0.0296(5) Uani 1 1 d . . . O33 O 0.70321(7) 0.59081(6) 0.37901(5) 0.0327(5) Uani 1 1 d . . . O34 O 0.68716(6) 0.61857(6) 0.47106(5) 0.0217(4) Uani 1 1 d . . . O35 O 0.77290(5) 0.67733(6) 0.46333(5) 0.0184(4) Uani 1 1 d . . . O36 O 0.79431(6) 0.56874(6) 0.48505(5) 0.0293(5) Uani 1 1 d . . . O37 O 0.73727(6) 0.58873(6) 0.55387(5) 0.0295(5) Uani 1 1 d . . . O38 O 0.83175(6) 0.66437(6) 0.55379(5) 0.0264(4) Uani 1 1 d . . . O39 O 0.80285(6) 0.69473(6) 0.64045(5) 0.0321(5) Uani 1 1 d . . . O40 O 0.90140(6) 0.74459(6) 0.62682(5) 0.0323(5) Uani 1 1 d . . . O41 O 0.79953(6) 0.79694(6) 0.61510(5) 0.0221(4) Uani 1 1 d . . . O42 O 0.73717(6) 0.70782(6) 0.54634(5) 0.0211(4) Uani 1 1 d . . . O43 O 0.67141(5) 0.72914(6) 0.46191(4) 0.0161(4) Uani 1 1 d . . . O44 O 0.82884(6) 0.77094(6) 0.53769(5) 0.0200(4) Uani 1 1 d . . . O45 O 0.76326(6) 0.79255(6) 0.45360(5) 0.0191(4) Uani 1 1 d . . . O46 O 0.72761(6) 0.82257(6) 0.53687(5) 0.0197(4) Uani 1 1 d . . . O47 O 0.79709(7) 0.90941(6) 0.62152(5) 0.0309(5) Uani 1 1 d . . . O48 O 0.89422(6) 0.86497(7) 0.60563(5) 0.0297(5) Uani 1 1 d . . . O49 O 0.70589(7) 0.93133(6) 0.51525(6) 0.0337(5) Uani 1 1 d . . . O50 O 0.76319(7) 0.91174(7) 0.44641(5) 0.0309(5) Uani 1 1 d . . . O51 O 0.81288(6) 0.88140(6) 0.52925(5) 0.0261(5) Uani 1 1 d . . . O52 O 0.66826(6) 0.83604(6) 0.44580(5) 0.0223(4) Uani 1 1 d . . . O53 O 0.59790(7) 0.75602(7) 0.37313(5) 0.0333(5) Uani 1 1 d . . . O54 O 0.69753(7) 0.80492(7) 0.35951(5) 0.0306(5) Uani 1 1 d . . . O55 O 0.52831(6) 0.79209(7) 0.51010(6) 0.0386(5) Uani 1 1 d . . . O56 O 0.55674(6) 0.86621(7) 0.61265(6) 0.0431(6) Uani 1 1 d . . . H56B H 0.5684 0.8994 0.6140 0.065 Uiso 1 1 calc R C 1 O57 O 0.46861(7) 0.89326(6) 0.58830(6) 0.0377(5) Uani 1 1 d . . . O58 O 0.97182(6) 0.70805(6) 0.48984(5) 0.0318(5) Uani 1 1 d . . . O59 O 0.94302(7) 0.63426(6) 0.38718(6) 0.0354(5) Uani 1 1 d . . . H59B H 0.9304 0.6011 0.3853 0.053 Uiso 1 1 calc R D 1 O60 O 1.03266(7) 0.60613(7) 0.41149(6) 0.0393(5) Uani 1 1 d . . . O61 O 0.15725(8) 0.78259(8) 0.88801(8) 0.0750(8) Uani 1 1 d . . . O62 O 0.60485(8) 0.96463(7) 0.61743(7) 0.0557(6) Uani 1 1 d . . . O63 O 0.71375(10) 0.96878(10) 0.31560(8) 0.0834(9) Uani 1 1 d . . . O64 O 0.34229(8) 0.71706(8) 0.11131(9) 0.0774(8) Uani 1 1 d . . . O65 O 0.89528(8) 0.53537(8) 0.38257(8) 0.0640(7) Uani 1 1 d . . . O66 O 0.78627(9) 0.53049(9) 0.68452(8) 0.0762(8) Uani 1 1 d . . . O67 O 0.08763(16) 0.68762(16) 0.64604(13) 0.0565(11) Uiso 0.50 1 d P E 1 O68 O 0.41612(16) 0.81560(16) 0.34780(13) 0.0534(11) Uiso 0.50 1 d P F 1 O69 O 0.89514(11) 0.76923(12) 0.34659(9) 0.1044(9) Uiso 1 1 d D G 1 O70 O 0.84612(12) 0.15015(11) 0.43461(8) 0.1090(10) Uani 1 1 d . H 1 O71 O 0.36611(9) 0.48598(11) 0.21574(10) 0.1056(11) Uani 1 1 d . I 1 O72 O 0.13527(11) 0.01274(12) 0.78289(7) 0.0969(10) Uani 1 1 d . J 1 O73 O 0.6441(2) 0.78195(19) 0.86395(13) 0.0795(17) Uani 0.50 1 d P K 1 O74 O 0.8581(2) 0.7217(2) 0.13305(16) 0.092(2) Uani 0.50 1 d P L 1 O75 O 0.65528(12) 0.35042(13) 0.56347(10) 0.0291(8) Uiso 0.50 1 d P M 1 O76 O 0.60441(10) 0.73025(10) 0.65233(8) 0.0526(7) Uiso 0.80 1 d P N 1 N1 N -0.15840(7) 0.99753(8) 0.05472(6) 0.0256(5) Uani 1 1 d . O 1 H1 H -0.1551 0.9811 0.0786 0.031 Uiso 1 1 calc R O 1 N2 N 0.65874(7) 0.50216(8) -0.05436(6) 0.0250(6) Uani 1 1 d . P 1 H2 H 0.6548 0.5181 -0.0786 0.030 Uiso 1 1 calc R P 1 N3 N 0.59542(7) 0.75180(7) 0.55901(6) 0.0236(5) Uani 1 1 d . Q 1 H3 H 0.6004 0.7376 0.5843 0.028 Uiso 1 1 calc R Q 1 N4 N 0.90492(7) 0.74765(7) 0.44091(6) 0.0209(5) Uani 1 1 d . R 1 H4 H 0.8999 0.7609 0.4152 0.025 Uiso 1 1 calc R R 1 N5 N 0.92659(9) 0.92313(8) 0.74262(7) 0.0393(7) Uani 1 1 d . S 1 N6 N 0.57511(9) 0.57655(9) 0.25724(7) 0.0423(7) Uani 1 1 d . T 1 N7 N 0.64105(9) 0.27525(8) 0.10531(8) 0.0467(7) Uani 1 1 d . U 1 N8 N 0.85858(9) 0.22455(9) 0.89519(9) 0.0517(8) Uani 1 1 d . V 1 N9 N 0.56254(7) 0.94089(7) 0.37810(7) 0.0274(6) Uani 1 1 d . W 1 N10 N 0.93677(8) 0.55919(8) 0.62206(6) 0.0283(6) Uani 1 1 d . X 1 N11 N 0.07188(8) 0.72812(8) 0.87421(8) 0.0418(7) Uani 1 1 d . Y 1 N12 N 0.68273(8) 1.02062(8) 0.61657(7) 0.0335(6) Uani 1 1 d . Z 1 N13 N 0.77456(9) 0.90160(10) 0.31325(8) 0.0551(8) Uani 1 1 d . A 1 N14 N 0.42808(9) 0.77088(9) 0.12510(7) 0.0425(7) Uani 1 1 d . B 1 N15 N 0.81726(9) 0.47814(8) 0.38356(8) 0.0411(7) Uani 1 1 d . C 1 N16 N 0.72637(10) 0.59725(10) 0.68607(8) 0.0505(8) Uani 1 1 d . D 1 N17 N 0.0391(4) 0.7999(4) 0.6268(3) 0.077(3) Uiso 0.30 1 d P E 2 N18 N 0.42689(19) 0.72909(19) 0.35519(15) 0.0270(11) Uiso 0.40 1 d P F 1 N19 N 0.9199(2) 0.7230(2) 0.27631(17) 0.0671(15) Uiso 0.50 1 d PD F 2 C1 C -0.07132(8) 0.95646(8) 0.05657(8) 0.0263(6) Uani 1 1 d U G 1 H1A H -0.0624 0.9667 0.0913 0.032 Uiso 1 1 calc R G 1 H1B H -0.0961 0.9202 0.0461 0.032 Uiso 1 1 calc R G 1 C2 C -0.12718(9) 0.98419(11) -0.01829(8) 0.0334(7) Uani 1 1 d U G 1 H2A H -0.1510 0.9474 -0.0277 0.040 Uiso 1 1 calc R G 1 H2B H -0.1529 1.0114 -0.0296 0.040 Uiso 1 1 calc R G 1 C3 C 0.07450(9) 0.94028(9) -0.05301(8) 0.0267(7) Uani 1 1 d U . 1 H3A H 0.0652 0.9304 -0.0878 0.032 Uiso 1 1 calc R . 1 H3B H 0.1012 0.9144 -0.0406 0.032 Uiso 1 1 calc R . 1 C4 C -0.10630(8) 1.00017(9) 0.03579(7) 0.0220(6) Uani 1 1 d U . 1 C5 C -0.21003(9) 1.01671(9) 0.04053(8) 0.0264(5) Uiso 1 1 d . O 1 C6 C -0.25528(9) 1.00247(9) 0.06569(8) 0.0258(7) Uani 1 1 d U O 1 C7 C -0.27530(10) 0.94657(10) 0.06254(8) 0.0302(6) Uiso 1 1 d . O 1 C8 C -0.31706(9) 0.93364(9) 0.08726(7) 0.0271(7) Uani 1 1 d U O 1 C9 C -0.33689(8) 0.97744(9) 0.11457(7) 0.0234(6) Uani 1 1 d U O 1 C10 C -0.31792(8) 1.03347(9) 0.11715(8) 0.0254(6) Uani 1 1 d U O 1 C11 C -0.27744(9) 1.04497(9) 0.09213(8) 0.0250(6) Uani 1 1 d U O 1 C12 C -0.25714(9) 1.10520(10) 0.09252(8) 0.0306(7) Uani 1 1 d U O 1 C13 C -0.25502(9) 0.90186(9) 0.03151(8) 0.0301(7) Uani 1 1 d U O 1 C14 C -0.26587(11) 0.90096(11) -0.01638(9) 0.0416(8) Uani 1 1 d U O 1 H14 H -0.2889 0.9273 -0.0288 0.050 Uiso 1 1 calc R O 1 C15 C -0.24434(11) 0.86305(11) -0.04656(11) 0.0565(10) Uani 1 1 d U O 1 H15 H -0.2517 0.8644 -0.0789 0.068 Uiso 1 1 calc R O 1 C16 C -0.21331(12) 0.82485(12) -0.03022(10) 0.0525(8) Uiso 1 1 d . O 1 H16 H -0.1995 0.7980 -0.0509 0.063 Uiso 1 1 calc R O 1 C17 C -0.20137(12) 0.82447(13) 0.01699(10) 0.0581(8) Uiso 1 1 d . O 1 H17 H -0.1776 0.7981 0.0285 0.070 Uiso 1 1 calc R O 1 C18 C -0.22306(10) 0.86171(10) 0.04896(9) 0.0405(7) Uiso 1 1 d . O 1 H18 H -0.2161 0.8595 0.0811 0.049 Uiso 1 1 calc R O 1 C19 C -0.33913(9) 0.87521(8) 0.08549(8) 0.0272(7) Uani 1 1 d U O 1 C20 C -0.37191(9) 0.84167(9) 0.04295(9) 0.0363(8) Uani 1 1 d U O 1 H20 H -0.3799 0.8549 0.0146 0.044 Uiso 1 1 calc R O 1 C21 C -0.39322(11) 0.78596(11) 0.04399(10) 0.0475(7) Uiso 1 1 d . O 1 H21 H -0.4163 0.7622 0.0158 0.057 Uiso 1 1 calc R O 1 C22 C -0.38078(11) 0.76654(12) 0.08504(9) 0.0485(7) Uiso 1 1 d . O 1 H22 H -0.3939 0.7296 0.0854 0.058 Uiso 1 1 calc R O 1 C23 C -0.34998(12) 0.80111(10) 0.12369(10) 0.0499(9) Uani 1 1 d U O 1 H23 H -0.3424 0.7883 0.1522 0.060 Uiso 1 1 calc R O 1 C24 C -0.32848(10) 0.85383(10) 0.12538(9) 0.0391(6) Uiso 1 1 d . O 1 H24X H -0.3058 0.8762 0.1544 0.047 Uiso 1 1 calc R O 1 C25 C -0.37937(9) 0.96467(9) 0.14162(8) 0.0312(7) Uani 1 1 d U O 1 C26 C -0.36382(11) 0.97306(10) 0.19127(9) 0.0401(8) Uani 1 1 d U O 1 H26 H -0.3247 0.9878 0.2084 0.048 Uiso 1 1 calc R O 1 C27 C -0.40410(12) 0.96036(10) 0.21528(9) 0.0494(8) Uani 1 1 d U O 1 H27 H -0.3920 0.9647 0.2485 0.059 Uiso 1 1 calc R O 1 C28 C -0.46158(12) 0.94144(11) 0.19171(11) 0.0670(10) Uani 1 1 d U O 1 H28 H -0.4897 0.9336 0.2083 0.080 Uiso 1 1 calc R O 1 C29 C -0.47732(12) 0.93415(12) 0.14384(11) 0.0605(11) Uani 1 1 d U O 1 H29 H -0.5171 0.9217 0.1272 0.073 Uiso 1 1 calc R O 1 C30 C -0.43668(10) 0.94452(10) 0.11892(8) 0.0396(8) Uani 1 1 d U O 1 H30 H -0.4488 0.9375 0.0855 0.048 Uiso 1 1 calc R O 1 C31 C -0.29998(12) 1.11273(11) 0.18643(9) 0.0464(7) Uiso 1 1 d . O 1 H31 H -0.2588 1.1106 0.1944 0.056 Uiso 1 1 calc R O 1 C32 C -0.32762(12) 1.15157(12) 0.21463(10) 0.0552(8) Uiso 1 1 d . O 1 H32 H -0.3037 1.1753 0.2425 0.066 Uiso 1 1 calc R O 1 C33 C -0.38623(12) 1.15535(12) 0.20274(10) 0.0568(8) Uiso 1 1 d . O 1 H33 H -0.4025 1.1805 0.2229 0.068 Uiso 1 1 calc R O 1 C34 C -0.42109(13) 1.12456(12) 0.16347(10) 0.0551(8) Uiso 1 1 d . O 1 H34 H -0.4616 1.1293 0.1541 0.066 Uiso 1 1 calc R O 1 C35 C -0.39744(11) 1.08569(12) 0.13668(10) 0.0474(7) Uiso 1 1 d . O 1 H35 H -0.4230 1.0621 0.1095 0.057 Uiso 1 1 calc R O 1 C36 C -0.33820(10) 1.07905(10) 0.14715(8) 0.0296(5) Uiso 1 1 d . O 1 C37 C 0.62812(9) 0.51590(9) 0.01896(7) 0.0232(5) Uiso 1 1 d . H 1 H37A H 0.6540 0.4890 0.0307 0.028 Uiso 1 1 calc R H 1 H37B H 0.6516 0.5528 0.0281 0.028 Uiso 1 1 calc R H 1 C38 C 0.42925(9) 0.45745(9) 0.05616(7) 0.0240(7) Uani 1 1 d U . 1 H38A H 0.4384 0.4687 0.0909 0.029 Uiso 1 1 calc R . 1 H38B H 0.4048 0.4210 0.0466 0.029 Uiso 1 1 calc R . 1 C39 C 0.57504(8) 0.44046(9) -0.05271(7) 0.0222(6) Uani 1 1 d U . 1 H39A H 0.5661 0.4316 -0.0875 0.027 Uiso 1 1 calc R . 1 H39B H 0.6014 0.4140 -0.0408 0.027 Uiso 1 1 calc R . 1 C40 C 0.60728(9) 0.49941(9) -0.03431(8) 0.0227(6) Uani 1 1 d U . 1 C41 C 0.71087(9) 0.48322(9) -0.03993(8) 0.0262(6) Uani 1 1 d U P 1 C42 C 0.75536(9) 0.49846(9) -0.06563(8) 0.0242(6) Uani 1 1 d U P 1 C43 C 0.77696(9) 0.55372(9) -0.06200(8) 0.0226(6) Uani 1 1 d U P 1 C44 C 0.81729(9) 0.56486(9) -0.08763(8) 0.0225(6) Uani 1 1 d U P 1 C45 C 0.83781(10) 0.52218(9) -0.11553(8) 0.0287(7) Uani 1 1 d U P 1 C46 C 0.81714(10) 0.46639(9) -0.11694(8) 0.0253(7) Uani 1 1 d U P 1 C47 C 0.77627(9) 0.45444(9) -0.09215(7) 0.0234(5) Uiso 1 1 d . P 1 C48 C 0.75610(10) 0.39637(9) -0.09242(9) 0.0325(7) Uani 1 1 d U P 1 C49 C 0.75567(10) 0.59843(10) -0.03131(9) 0.0344(8) Uani 1 1 d U P 1 C50 C 0.72382(11) 0.63718(11) -0.04969(10) 0.0451(7) Uiso 1 1 d . P 1 H50 H 0.7180 0.6362 -0.0823 0.054 Uiso 1 1 calc R P 1 C51 C 0.69981(13) 0.67718(14) -0.02424(11) 0.0668(10) Uiso 1 1 d . P 1 H51 H 0.6777 0.7030 -0.0384 0.080 Uiso 1 1 calc R P 1 C52 C 0.70945(14) 0.67770(14) 0.02217(12) 0.0677(10) Uiso 1 1 d . P 1 H52 H 0.6936 0.7053 0.0406 0.081 Uiso 1 1 calc R P 1 C53 C 0.74039(12) 0.64134(15) 0.04471(10) 0.0745(12) Uani 1 1 d U P 1 H53 H 0.7454 0.6435 0.0774 0.089 Uiso 1 1 calc R P 1 C54 C 0.76537(10) 0.59909(11) 0.01656(9) 0.0420(8) Uani 1 1 d U P 1 H54 H 0.7874 0.5730 0.0304 0.050 Uiso 1 1 calc R P 1 C55 C 0.82899(10) 0.64665(10) -0.12481(9) 0.0371(7) Uani 1 1 d U P 1 H55 H 0.8074 0.6246 -0.1543 0.044 Uiso 1 1 calc R P 1 C56 C 0.85061(11) 0.70266(11) -0.12195(10) 0.0576(9) Uani 1 1 d U P 1 H56 H 0.8421 0.7188 -0.1488 0.069 Uiso 1 1 calc R P 1 C57 C 0.88483(11) 0.73332(12) -0.07824(9) 0.0440(7) Uiso 1 1 d . P 1 H57 H 0.9021 0.7699 -0.0760 0.053 Uiso 1 1 calc R P 1 C58 C 0.89365(10) 0.71133(11) -0.03879(9) 0.0384(7) Uiso 1 1 d . P 1 H58 H 0.9149 0.7331 -0.0090 0.046 Uiso 1 1 calc R P 1 C59 C 0.87155(10) 0.65782(10) -0.04290(9) 0.0390(8) Uani 1 1 d U P 1 H59 H 0.8786 0.6427 -0.0155 0.047 Uiso 1 1 calc R P 1 C60 C 0.83887(9) 0.62406(10) -0.08562(8) 0.0305(7) Uani 1 1 d U P 1 C61 C 0.88127(10) 0.53574(10) -0.14146(8) 0.0318(7) Uani 1 1 d U P 1 C62 C 0.86289(10) 0.52608(10) -0.19041(8) 0.0364(7) Uani 1 1 d U P 1 H62 H 0.8234 0.5109 -0.2061 0.044 Uiso 1 1 calc R P 1 C63 C 0.90093(12) 0.53816(11) -0.21641(10) 0.0504(10) Uani 1 1 d U P 1 H63 H 0.8875 0.5334 -0.2496 0.060 Uiso 1 1 calc R P 1 C64 C 0.95879(13) 0.55730(12) -0.19350(9) 0.0567(9) Uani 1 1 d U P 1 H64 H 0.9854 0.5652 -0.2113 0.068 Uiso 1 1 calc R P 1 C65 C 0.97917(11) 0.56540(12) -0.14498(11) 0.0578(10) Uani 1 1 d U P 1 H65 H 1.0195 0.5776 -0.1299 0.069 Uiso 1 1 calc R P 1 C66 C 0.93996(10) 0.55548(11) -0.11880(10) 0.0433(9) Uani 1 1 d U P 1 H66 H 0.9531 0.5621 -0.0855 0.052 Uiso 1 1 calc R P 1 C67 C 0.83967(10) 0.42089(10) -0.14600(8) 0.0318(6) Uiso 1 1 d . P 1 C68 C 0.89841(9) 0.41264(9) -0.13767(9) 0.0401(7) Uani 1 1 d U P 1 H68 H 0.9266 0.4336 -0.1106 0.048 Uiso 1 1 calc R P 1 C69 C 0.91541(12) 0.37191(12) -0.17078(10) 0.0491(8) Uiso 1 1 d . P 1 H69 H 0.9555 0.3658 -0.1662 0.059 Uiso 1 1 calc R P 1 C70 C 0.87319(11) 0.34110(12) -0.20985(10) 0.0476(7) Uiso 1 1 d . P 1 H70 H 0.8853 0.3146 -0.2319 0.057 Uiso 1 1 calc R P 1 C71 C 0.81479(11) 0.34792(11) -0.21741(9) 0.0461(7) Uiso 1 1 d . P 1 H71 H 0.7857 0.3260 -0.2434 0.055 Uiso 1 1 calc R P 1 C72 C 0.80115(13) 0.38824(10) -0.18517(9) 0.0469(8) Uani 1 1 d U P 1 H72 H 0.7610 0.3943 -0.1904 0.056 Uiso 1 1 calc R P 1 C73 C 0.87642(8) 0.76555(9) 0.51512(7) 0.0238(6) Uani 1 1 d U R 1 H73A H 0.9017 0.7389 0.5280 0.029 Uiso 1 1 calc R R 1 H73B H 0.9008 0.8018 0.5224 0.029 Uiso 1 1 calc R R 1 C74 C 0.81685(9) 0.78693(9) 0.43968(7) 0.0240(6) Uani 1 1 d U R 1 H74A H 0.8405 0.8237 0.4483 0.029 Uiso 1 1 calc R R 1 H74B H 0.8072 0.7748 0.4050 0.029 Uiso 1 1 calc R R 1 C75 C 0.85449(8) 0.74579(9) 0.46172(7) 0.0198(5) Uiso 1 1 d . R 1 C76 C 0.82441(8) 0.68530(8) 0.44650(7) 0.0204(6) Uani 1 1 d U R 1 H76A H 0.8132 0.6745 0.4117 0.025 Uiso 1 1 calc R R 1 H76B H 0.8530 0.6606 0.4585 0.025 Uiso 1 1 calc R R 1 C77 C 0.95790(9) 0.73120(8) 0.45702(7) 0.0218(6) Uani 1 1 d U R 1 C78 C 1.02497(9) 0.79941(9) 0.43453(7) 0.0271(6) Uani 1 1 d U R 1 C79 C 1.07011(9) 0.81118(9) 0.41362(7) 0.0251(5) Uiso 1 1 d . R 1 C80 C 1.09393(9) 0.76707(9) 0.38943(7) 0.0206(6) Uani 1 1 d U R 1 C81 C 1.07092(9) 0.71194(9) 0.38521(7) 0.0260(6) Uani 1 1 d U R 1 C82 C 1.02559(9) 0.70081(9) 0.40608(7) 0.0239(5) Uiso 1 1 d . R 1 C83 C 1.00247(9) 0.74378(8) 0.43087(8) 0.0242(6) Uani 1 1 d U R 1 C84 C 1.00313(9) 0.64156(10) 0.40308(8) 0.0297(7) Uani 1 1 d U R 1 C85 C 1.00031(9) 0.84475(9) 0.46111(9) 0.0306(7) Uani 1 1 d U R 1 C86 C 0.96960(11) 0.88036(11) 0.43819(10) 0.0534(9) Uani 1 1 d U R 1 H86 H 0.9651 0.8754 0.4052 0.064 Uiso 1 1 calc R R 1 C87 C 0.94428(13) 0.92394(13) 0.46019(11) 0.0621(9) Uiso 1 1 d . R 1 H87 H 0.9231 0.9478 0.4428 0.075 Uiso 1 1 calc R R 1 C88 C 0.95125(13) 0.93071(13) 0.50763(11) 0.0621(9) Uiso 1 1 d . R 1 H88 H 0.9354 0.9603 0.5238 0.075 Uiso 1 1 calc R R 1 C89 C 0.97989(12) 0.89648(12) 0.53117(10) 0.0517(8) Uiso 1 1 d . R 1 H89 H 0.9825 0.9009 0.5638 0.062 Uiso 1 1 calc R R 1 C90 C 1.00723(11) 0.85283(9) 0.50866(9) 0.0366(8) Uani 1 1 d U R 1 H90 H 1.0297 0.8300 0.5265 0.044 Uiso 1 1 calc R R 1 C91 C 1.09428(9) 0.86997(9) 0.41807(8) 0.0247(6) Uani 1 1 d U R 1 C92 C 1.09010(10) 0.89299(10) 0.37915(9) 0.0375(8) Uani 1 1 d U R 1 H92 H 1.0714 0.8714 0.3487 0.045 Uiso 1 1 calc R R 1 C93 C 1.11333(10) 0.94821(9) 0.38426(9) 0.0421(7) Uani 1 1 d U R 1 H93 H 1.1113 0.9633 0.3571 0.051 Uiso 1 1 calc R R 1 C94 C 1.13884(10) 0.98053(10) 0.42779(9) 0.0424(8) Uani 1 1 d U R 1 H94 H 1.1533 1.0182 0.4312 0.051 Uiso 1 1 calc R R 1 C95 C 1.14332(10) 0.95746(11) 0.46679(9) 0.0434(8) Uani 1 1 d U R 1 H95 H 1.1618 0.9793 0.4972 0.052 Uiso 1 1 calc R R 1 C96 C 1.12137(9) 0.90324(9) 0.46219(9) 0.0302(7) Uani 1 1 d U R 1 H96 H 1.1247 0.8882 0.4895 0.036 Uiso 1 1 calc R R 1 C97 C 1.14390(8) 0.77923(8) 0.36801(8) 0.0257(7) Uani 1 1 d U R 1 C98 C 1.13838(10) 0.77136(9) 0.32094(7) 0.0307(7) Uani 1 1 d U R 1 H98 H 1.1010 0.7585 0.2996 0.037 Uiso 1 1 calc R R 1 C99 C 1.18594(11) 0.78172(10) 0.30396(8) 0.0453(8) Uani 1 1 d U R 1 H99 H 1.1812 0.7767 0.2710 0.054 Uiso 1 1 calc R R 1 C100 C 1.24215(10) 0.79987(10) 0.33524(10) 0.0494(8) Uani 1 1 d U R 1 H100 H 1.2756 0.8062 0.3236 0.059 Uiso 1 1 calc R R 1 C101 C 1.24721(10) 0.80784(10) 0.38113(9) 0.0391(8) Uani 1 1 d U R 1 H101 H 1.2847 0.8208 0.4023 0.047 Uiso 1 1 calc R R 1 C102 C 1.19980(10) 0.79789(9) 0.39924(8) 0.0322(7) Uani 1 1 d U R 1 H102 H 1.2048 0.8036 0.4323 0.039 Uiso 1 1 calc R R 1 C103 C 1.09752(9) 0.66593(9) 0.35989(7) 0.0268(6) Uani 1 1 d U R 1 C104 C 1.06677(11) 0.63669(10) 0.31640(9) 0.0406(8) Uani 1 1 d U R 1 H104 H 1.0288 0.6449 0.3021 0.049 Uiso 1 1 calc R R 1 C105 C 1.09235(13) 0.59452(12) 0.29345(11) 0.0631(10) Uani 1 1 d U R 1 H105 H 1.0698 0.5724 0.2642 0.076 Uiso 1 1 calc R R 1 C106 C 1.14696(12) 0.58380(11) 0.31062(10) 0.0637(9) Uani 1 1 d U R 1 H106 H 1.1647 0.5571 0.2930 0.076 Uiso 1 1 calc R R 1 C107 C 1.17544(14) 0.61180(13) 0.35314(11) 0.0654(9) Uiso 1 1 d . R 1 H107 H 1.2131 0.6022 0.3666 0.078 Uiso 1 1 calc R R 1 C108 C 1.15398(10) 0.65498(10) 0.38001(9) 0.0383(6) Uiso 1 1 d . R 1 H108 H 1.1766 0.6753 0.4099 0.046 Uiso 1 1 calc R R 1 C109 C 0.68310(9) 0.71226(9) 0.56003(8) 0.0226(6) Uani 1 1 d U Q 1 H10A H 0.6922 0.7233 0.5947 0.027 Uiso 1 1 calc R Q 1 H10B H 0.6595 0.6754 0.5503 0.027 Uiso 1 1 calc R Q 1 C110 C 0.67604(9) 0.81391(9) 0.55315(8) 0.0245(5) Uiso 1 1 d . Q 1 H11C H 0.6476 0.8387 0.5412 0.029 Uiso 1 1 calc R Q 1 H11D H 0.6871 0.8247 0.5879 0.029 Uiso 1 1 calc R Q 1 C111 C 0.62356(9) 0.73484(9) 0.48451(7) 0.0218(6) Uani 1 1 d U Q 1 H11E H 0.5990 0.6987 0.4772 0.026 Uiso 1 1 calc R Q 1 H11F H 0.5985 0.7617 0.4716 0.026 Uiso 1 1 calc R Q 1 C112 C 0.64576(9) 0.75469(9) 0.53834(7) 0.0223(6) Uani 1 1 d U Q 1 C113 C 0.54253(10) 0.76853(10) 0.54337(8) 0.0302(6) Uiso 1 1 d . Q 1 C114 C 0.49707(9) 0.75474(10) 0.56931(7) 0.0244(7) Uani 1 1 d U Q 1 C115 C 0.47361(9) 0.79891(9) 0.59404(8) 0.0240(6) Uani 1 1 d U Q 1 C116 C 0.42776(9) 0.78704(9) 0.61400(8) 0.0223(6) Uani 1 1 d U Q 1 C117 C 0.40518(9) 0.73164(9) 0.60990(8) 0.0246(7) Uani 1 1 d U Q 1 C118 C 0.42898(9) 0.68831(8) 0.58612(7) 0.0193(6) Uani 1 1 d U Q 1 C119 C 0.47519(9) 0.69927(8) 0.56506(8) 0.0242(6) Uani 1 1 d U Q 1 C120 C 0.50170(9) 0.65312(9) 0.54010(8) 0.0286(7) Uani 1 1 d U Q 1 C121 C 0.49319(10) 0.64773(11) 0.49160(9) 0.0405(8) Uani 1 1 d U Q 1 H1A1 H 0.4713 0.6727 0.4761 0.049 Uiso 1 1 calc R Q 1 C122 C 0.51597(11) 0.60683(11) 0.46621(10) 0.0480(8) Uiso 1 1 d . Q 1 H122 H 0.5107 0.6040 0.4334 0.058 Uiso 1 1 calc R Q 1 C123 C 0.54546(13) 0.57121(14) 0.48758(11) 0.0644(9) Uiso 1 1 d . Q 1 H123 H 0.5605 0.5425 0.4696 0.077 Uiso 1 1 calc R Q 1 C124 C 0.55470(13) 0.57505(14) 0.53551(11) 0.0627(9) Uiso 1 1 d . Q 1 H124 H 0.5763 0.5492 0.5501 0.075 Uiso 1 1 calc R Q 1 C125 C 0.53216(10) 0.61723(9) 0.56315(10) 0.0399(8) Uani 1 1 d U Q 1 H125 H 0.5380 0.6203 0.5961 0.048 Uiso 1 1 calc R Q 1 C126 C 0.40520(9) 0.62951(9) 0.58147(9) 0.0290(7) Uani 1 1 d U Q 1 C127 C 0.40918(9) 0.60789(9) 0.62150(8) 0.0298(7) Uani 1 1 d U Q 1 H127 H 0.4266 0.6305 0.6518 0.036 Uiso 1 1 calc R Q 1 C128 C 0.38781(11) 0.55362(11) 0.61708(10) 0.0438(9) Uani 1 1 d U Q 1 H128 H 0.3909 0.5391 0.6446 0.053 Uiso 1 1 calc R Q 1 C129 C 0.36272(11) 0.52072(11) 0.57497(10) 0.0470(9) Uani 1 1 d U Q 1 H129 H 0.3487 0.4832 0.5728 0.056 Uiso 1 1 calc R Q 1 C130 C 0.35728(10) 0.54108(9) 0.53486(10) 0.0373(8) Uani 1 1 d U Q 1 H130 H 0.3392 0.5179 0.5049 0.045 Uiso 1 1 calc R Q 1 C131 C 0.37834(10) 0.59580(10) 0.53843(9) 0.0344(8) Uani 1 1 d U Q 1 H131 H 0.3741 0.6102 0.5107 0.041 Uiso 1 1 calc R Q 1 C132 C 0.35471(9) 0.71991(9) 0.62900(7) 0.0227(6) Uani 1 1 d U Q 1 C133 C 0.36212(9) 0.72828(10) 0.67794(9) 0.0326(8) Uani 1 1 d U Q 1 H133 H 0.4000 0.7410 0.6987 0.039 Uiso 1 1 calc R Q 1 C134 C 0.31488(11) 0.71819(11) 0.69594(10) 0.0425(7) Uiso 1 1 d . Q 1 H134 H 0.3204 0.7233 0.7290 0.051 Uiso 1 1 calc R Q 1 C135 C 0.25936(11) 0.70069(11) 0.66602(9) 0.0411(7) Uiso 1 1 d . Q 1 H135 H 0.2268 0.6941 0.6786 0.049 Uiso 1 1 calc R Q 1 C136 C 0.25108(10) 0.69267(11) 0.61752(9) 0.0403(9) Uani 1 1 d U Q 1 H136 H 0.2129 0.6814 0.5969 0.048 Uiso 1 1 calc R Q 1 C137 C 0.29842(9) 0.70115(10) 0.59983(9) 0.0335(8) Uani 1 1 d U Q 1 H137 H 0.2928 0.6941 0.5667 0.040 Uiso 1 1 calc R Q 1 C138 C 0.43169(11) 0.86439(11) 0.68344(9) 0.0447(9) Uani 1 1 d U Q 1 H138 H 0.4704 0.8583 0.6982 0.054 Uiso 1 1 calc R Q 1 C139 C 0.40302(13) 0.90579(11) 0.70619(10) 0.0654(10) Uani 1 1 d U Q 1 H139 H 0.4223 0.9271 0.7366 0.078 Uiso 1 1 calc R Q 1 C140 C 0.34881(12) 0.91461(11) 0.68456(12) 0.0682(10) Uani 1 1 d U Q 1 H140 H 0.3305 0.9425 0.7003 0.082 Uiso 1 1 calc R Q 1 C141 C 0.31882(13) 0.88540(12) 0.64105(10) 0.0540(8) Uiso 1 1 d . Q 1 H141 H 0.2809 0.8930 0.6259 0.065 Uiso 1 1 calc R Q 1 C142 C 0.34654(12) 0.84403(12) 0.61999(10) 0.0515(8) Uiso 1 1 d . Q 1 H142 H 0.3258 0.8218 0.5903 0.062 Uiso 1 1 calc R Q 1 C143 C 0.40266(10) 0.83350(10) 0.63993(8) 0.0299(7) Uani 1 1 d U Q 1 C144 C 0.49867(10) 0.85776(9) 0.59740(7) 0.0260(6) Uani 1 1 d U Q 1 C145 C 0.94418(11) 0.93728(10) 0.70040(8) 0.0387(8) Uani 1 1 d U S 1 H14B H 0.9587 0.9044 0.6843 0.046 Uiso 1 1 calc R S 1 H14C H 0.9085 0.9446 0.6782 0.046 Uiso 1 1 calc R S 1 C146 C 0.99033(11) 0.98610(11) 0.71075(9) 0.0436(8) Uani 1 1 d U S 1 H14D H 1.0235 0.9833 0.7373 0.052 Uiso 1 1 calc R S 1 H14E H 0.9735 1.0209 0.7196 0.052 Uiso 1 1 calc R S 1 C147 C 1.01236(11) 0.98653(12) 0.66625(8) 0.0479(9) Uani 1 1 d U S 1 H14F H 1.0346 0.9546 0.6604 0.058 Uiso 1 1 calc R S 1 H14G H 0.9783 0.9830 0.6387 0.058 Uiso 1 1 calc R S 1 C148 C 1.05179(13) 1.04017(13) 0.67242(11) 0.0675(11) Uani 1 1 d U S 1 H14H H 1.0307 1.0718 0.6805 0.101 Uiso 1 1 calc R S 1 H14I H 1.0626 1.0414 0.6430 0.101 Uiso 1 1 calc R S 1 H14J H 1.0875 1.0418 0.6977 0.101 Uiso 1 1 calc R S 1 C149 C 0.97738(11) 0.90850(11) 0.77835(8) 0.0418(8) Uani 1 1 d U S 1 H14K H 1.0059 0.9421 0.7928 0.050 Uiso 1 1 calc R S 1 H14L H 0.9621 0.8972 0.8036 0.050 Uiso 1 1 calc R S 1 C150 C 1.00916(14) 0.86320(12) 0.75868(10) 0.0683(11) Uani 1 1 d U S 1 H15A H 1.0255 0.8746 0.7339 0.082 Uiso 1 1 calc R S 1 H15B H 0.9809 0.8295 0.7439 0.082 Uiso 1 1 calc R S 1 C151 C 1.05929(14) 0.84963(15) 0.79654(11) 0.0795(13) Uani 1 1 d U S 1 H15C H 1.0866 0.8837 0.8123 0.095 Uiso 1 1 calc R S 1 H15D H 1.0428 0.8365 0.8205 0.095 Uiso 1 1 calc R S 1 C152 C 1.0918(2) 0.8073(2) 0.77686(17) 0.0397(13) Uiso 0.50 1 d P S 1 H15E H 1.0644 0.7746 0.7588 0.060 Uiso 1 1 calc R S 1 H15F H 1.1205 0.7969 0.8024 0.060 Uiso 1 1 calc R S 1 H15G H 1.1125 0.8219 0.7561 0.060 Uiso 1 1 calc R S 1 C153 C 0.87783(11) 0.87416(10) 0.72317(8) 0.0395(8) Uani 1 1 d U S 1 H15H H 0.8442 0.8861 0.7020 0.047 Uiso 1 1 calc R S 1 H15I H 0.8927 0.8441 0.7039 0.047 Uiso 1 1 calc R S 1 C154 C 0.85564(13) 0.85089(12) 0.75944(9) 0.0554(10) Uani 1 1 d U S 1 H15J H 0.8449 0.8811 0.7815 0.066 Uiso 1 1 calc R S 1 H15K H 0.8869 0.8331 0.7777 0.066 Uiso 1 1 calc R S 1 C155 C 0.80186(13) 0.80825(14) 0.73495(11) 0.0699(10) Uiso 1 1 d . S 1 H15L H 0.7742 0.8243 0.7120 0.084 Uiso 1 1 calc R S 1 H15M H 0.8145 0.7753 0.7172 0.084 Uiso 1 1 calc R S 1 C156 C 0.7728(3) 0.7917(3) 0.7660(2) 0.089(2) Uiso 0.50 1 d P S 1 H15N H 0.7473 0.7570 0.7506 0.134 Uiso 1 1 calc R S 1 H15O H 0.7490 0.8204 0.7757 0.134 Uiso 1 1 calc R S 1 H15P H 0.8017 0.7860 0.7938 0.134 Uiso 1 1 calc R S 1 C856 C 0.7472(3) 0.8285(3) 0.7135(3) 0.0295(18) Uiso 0.30 1 d P I 2 C157 C 0.90142(11) 0.97155(11) 0.76739(8) 0.0424(9) Uani 1 1 d U S 1 H15Q H 0.9341 1.0015 0.7832 0.051 Uiso 1 1 calc R S 1 H15R H 0.8860 0.9593 0.7922 0.051 Uiso 1 1 calc R S 1 C158 C 0.85241(12) 0.99607(13) 0.73658(10) 0.0598(11) Uani 1 1 d U S 1 H15S H 0.8702 1.0186 0.7183 0.072 Uiso 1 1 calc R S 1 H15T H 0.8253 0.9653 0.7138 0.072 Uiso 1 1 calc R S 1 C159 C 0.81704(13) 1.03185(14) 0.76362(11) 0.0774(13) Uani 1 1 d DU S 1 H15U H 0.8063 1.0117 0.7865 0.093 Uiso 1 1 calc R S 1 H15V H 0.8431 1.0659 0.7820 0.093 Uiso 1 1 calc R S 1 C160 C 0.7673(2) 1.0474(3) 0.7388(2) 0.0405(16) Uiso 0.40 1 d PD S 1 H16A H 0.7775 1.0779 0.7245 0.061 Uiso 0.40 1 calc PR S 1 H16B H 0.7425 1.0595 0.7598 0.061 Uiso 0.40 1 calc PR S 1 H16C H 0.7459 1.0159 0.7140 0.061 Uiso 0.40 1 calc PR S 1 C860 C 0.7643(4) 0.9895(4) 0.7685(3) 0.045(2) Uiso 0.30 1 d P J 2 C161 C 0.59909(11) 0.52752(11) 0.23199(9) 0.0402(8) Uani 1 1 d U T 1 H16D H 0.5662 0.4978 0.2165 0.048 Uiso 1 1 calc R T 1 H16E H 0.6147 0.5392 0.2070 0.048 Uiso 1 1 calc R T 1 C162 C 0.64646(13) 0.50434(13) 0.26289(10) 0.0647(11) Uani 1 1 d U T 1 H16F H 0.6284 0.4813 0.2807 0.078 Uiso 1 1 calc R T 1 H16G H 0.6730 0.5352 0.2859 0.078 Uiso 1 1 calc R T 1 C163 C 0.68170(13) 0.46999(15) 0.23586(11) 0.0737(13) Uani 1 1 d DU T 1 H16H H 0.6545 0.4394 0.2130 0.088 Uiso 1 1 calc R T 1 H16I H 0.6984 0.4933 0.2176 0.088 Uiso 1 1 calc R T 1 C164 C 0.7271(3) 0.4472(3) 0.2614(2) 0.0483(19) Uiso 0.40 1 d PD T 1 H16J H 0.7504 0.4756 0.2881 0.072 Uiso 0.40 1 calc PR T 1 H16K H 0.7522 0.4330 0.2412 0.072 Uiso 0.40 1 calc PR T 1 H16L H 0.7108 0.4168 0.2730 0.072 Uiso 0.40 1 calc PR T 1 C864 C 0.7360(4) 0.4978(4) 0.2341(3) 0.041(2) Uiso 0.30 1 d P K 2 C165 C 0.55631(11) 0.56383(11) 0.29959(8) 0.0389(8) Uani 1 1 d U T 1 H16M H 0.5404 0.5967 0.3142 0.047 Uiso 1 1 calc R T 1 H16N H 0.5917 0.5581 0.3230 0.047 Uiso 1 1 calc R T 1 C166 C 0.51039(11) 0.51338(12) 0.28942(9) 0.0491(10) Uani 1 1 d U T 1 H16O H 0.4768 0.5156 0.2629 0.059 Uiso 1 1 calc R T 1 H16P H 0.5280 0.4790 0.2806 0.059 Uiso 1 1 calc R T 1 C167 C 0.48927(13) 0.51224(12) 0.33301(11) 0.0586(11) Uani 1 1 d U T 1 H16Q H 0.4674 0.5444 0.3393 0.070 Uiso 1 1 calc R T 1 H16R H 0.5236 0.5155 0.3603 0.070 Uiso 1 1 calc R T 1 C168 C 0.44915(14) 0.45846(14) 0.32731(12) 0.0796(14) Uani 1 1 d U T 1 H16S H 0.4132 0.4570 0.3023 0.119 Uiso 1 1 calc R T 1 H16T H 0.4388 0.4576 0.3569 0.119 Uiso 1 1 calc R T 1 H16U H 0.4699 0.4265 0.3191 0.119 Uiso 1 1 calc R T 1 C169 C 0.62209(12) 0.62740(12) 0.27668(9) 0.0497(10) Uani 1 1 d U T 1 H16V H 0.6047 0.6578 0.2933 0.060 Uiso 1 1 calc R T 1 H16W H 0.6551 0.6178 0.3001 0.060 Uiso 1 1 calc R T 1 C170 C 0.64676(13) 0.64868(13) 0.23991(10) 0.0559(10) Uani 1 1 d U T 1 H17A H 0.6164 0.6660 0.2203 0.067 Uiso 1 1 calc R T 1 H17B H 0.6579 0.6174 0.2191 0.067 Uiso 1 1 calc R T 1 C171 C 0.70282(17) 0.69285(14) 0.26532(10) 0.1042(14) Uani 1 1 d U T 1 H17C H 0.6910 0.7251 0.2846 0.125 Uiso 1 1 calc R T 1 H17D H 0.7319 0.6761 0.2866 0.125 Uiso 1 1 calc R T 1 C172 C 0.7294(2) 0.7113(3) 0.2312(2) 0.0353(15) Uiso 0.40 1 d P T 1 H17E H 0.7212 0.6821 0.2027 0.053 Uiso 0.40 1 calc PR T 1 H17F H 0.7721 0.7197 0.2445 0.053 Uiso 0.40 1 calc PR T 1 H17G H 0.7131 0.7447 0.2235 0.053 Uiso 0.40 1 calc PR T 1 C872 C 0.7560(4) 0.6727(4) 0.2923(3) 0.086(3) Uiso 0.40 1 d P L 2 C173 C 0.52514(12) 0.58996(12) 0.22234(9) 0.0518(10) Uani 1 1 d U T 1 H17H H 0.4966 0.5562 0.2088 0.062 Uiso 1 1 calc R T 1 H17I H 0.5400 0.6001 0.1965 0.062 Uiso 1 1 calc R T 1 C174 C 0.49289(13) 0.63649(13) 0.24125(10) 0.0629(11) Uani 1 1 d U T 1 H17J H 0.4767 0.6262 0.2665 0.075 Uiso 1 1 calc R T 1 H17K H 0.5211 0.6704 0.2552 0.075 Uiso 1 1 calc R T 1 C175 C 0.44397(13) 0.64855(14) 0.20395(12) 0.0762(13) Uani 1 1 d DU T 1 H17L H 0.4178 0.6138 0.1879 0.091 Uiso 1 1 calc R T 1 H17M H 0.4606 0.6622 0.1803 0.091 Uiso 1 1 calc R T 1 C176 C 0.40714(14) 0.69228(15) 0.22390(14) 0.1105(15) Uani 1 1 d DU T 1 H17N H 0.4032 0.6866 0.2545 0.166 Uiso 1 1 calc R T 1 H17O H 0.3680 0.6883 0.2021 0.166 Uiso 1 1 calc R T 1 H17P H 0.4270 0.7296 0.2276 0.166 Uiso 1 1 calc R T 1 C177 C 0.61218(12) 0.21864(11) 0.07483(10) 0.0513(10) Uani 1 1 d U U 1 H17Q H 0.6418 0.2002 0.0610 0.062 Uiso 1 1 calc R U 1 H17R H 0.6000 0.1955 0.0953 0.062 Uiso 1 1 calc R U 1 C178 C 0.55858(13) 0.22121(12) 0.03509(12) 0.0630(11) Uani 1 1 d U U 1 H17S H 0.5264 0.2350 0.0484 0.076 Uiso 1 1 calc R U 1 H17T H 0.5690 0.2471 0.0161 0.076 Uiso 1 1 calc R U 1 C179 C 0.53838(14) 0.16379(15) 0.00432(12) 0.0856(15) Uani 1 1 d DU U 1 H17U H 0.5011 0.1644 -0.0193 0.103 Uiso 1 1 calc R U 1 H17V H 0.5308 0.1376 0.0240 0.103 Uiso 1 1 calc R U 1 C180 C 0.5847(2) 0.1440(2) -0.02082(16) 0.160(3) Uani 1 1 d DU U 1 H18A H 0.5919 0.1697 -0.0405 0.241 Uiso 1 1 calc R U 1 H18B H 0.5705 0.1069 -0.0406 0.241 Uiso 1 1 calc R U 1 H18C H 0.6213 0.1425 0.0025 0.241 Uiso 1 1 calc R U 1 C181 C 0.66335(12) 0.31145(11) 0.07566(11) 0.0608(11) Uani 1 1 d U U 1 H18D H 0.6287 0.3207 0.0536 0.073 Uiso 1 1 calc R U 1 H18E H 0.6837 0.3466 0.0969 0.073 Uiso 1 1 calc R U 1 C182 C 0.70475(16) 0.28770(16) 0.04729(15) 0.1241(17) Uani 1 1 d U U 1 H18F H 0.6858 0.2517 0.0266 0.149 Uiso 1 1 calc R U 1 H18G H 0.7411 0.2809 0.0690 0.149 Uiso 1 1 calc R U 1 C183 C 0.72094(18) 0.32696(18) 0.01701(15) 0.0759(13) Uiso 0.80 1 d P U 1 H18H H 0.7321 0.3064 -0.0107 0.091 Uiso 0.80 1 calc PR U 1 H18I H 0.6880 0.3481 0.0062 0.091 Uiso 0.80 1 calc PR U 1 C184 C 0.7635(3) 0.3579(3) 0.0448(3) 0.060(2) Uiso 0.40 1 d P U 1 H18J H 0.7494 0.3897 0.0620 0.091 Uiso 0.40 1 calc PR U 1 H18K H 0.7898 0.3710 0.0272 0.091 Uiso 0.40 1 calc PR U 1 H18L H 0.7850 0.3375 0.0671 0.091 Uiso 0.40 1 calc PR U 1 C185 C 0.59879(11) 0.30704(11) 0.12757(11) 0.0536(10) Uani 1 1 d U U 1 H18M H 0.5674 0.3155 0.1022 0.064 Uiso 1 1 calc R U 1 H18N H 0.6202 0.3428 0.1471 0.064 Uiso 1 1 calc R U 1 C186 C 0.57020(13) 0.27767(12) 0.15802(11) 0.0644(11) Uani 1 1 d U U 1 H18O H 0.6018 0.2706 0.1839 0.077 Uiso 1 1 calc R U 1 H18P H 0.5506 0.2412 0.1388 0.077 Uiso 1 1 calc R U 1 C187 C 0.52262(16) 0.30858(15) 0.18094(18) 0.149(2) Uani 1 1 d U U 1 H18Q H 0.4944 0.3230 0.1572 0.179 Uiso 1 1 calc R U 1 H18R H 0.5006 0.2830 0.1942 0.179 Uiso 1 1 calc R U 1 C188 C 0.5573(2) 0.35308(19) 0.21734(19) 0.173(2) Uani 1 1 d U U 1 H18S H 0.5863 0.3380 0.2395 0.260 Uiso 1 1 calc R U 1 H18T H 0.5315 0.3732 0.2341 0.260 Uiso 1 1 calc R U 1 H18U H 0.5776 0.3785 0.2033 0.260 Uiso 1 1 calc R U 1 C189 C 0.69111(12) 0.26216(11) 0.14154(11) 0.0536(10) Uani 1 1 d U U 1 H18V H 0.7165 0.2405 0.1249 0.064 Uiso 1 1 calc R U 1 H18W H 0.6746 0.2379 0.1592 0.064 Uiso 1 1 calc R U 1 C190 C 0.72945(13) 0.31023(13) 0.17655(12) 0.0689(12) Uani 1 1 d U U 1 H19A H 0.7059 0.3305 0.1959 0.083 Uiso 1 1 calc R U 1 H19B H 0.7451 0.3361 0.1597 0.083 Uiso 1 1 calc R U 1 C191 C 0.78003(13) 0.28964(13) 0.20808(10) 0.0595(11) Uani 1 1 d U U 1 H19C H 0.8013 0.2667 0.1882 0.071 Uiso 1 1 calc R U 1 H19D H 0.7640 0.2658 0.2263 0.071 Uiso 1 1 calc R U 1 C192 C 0.82320(14) 0.33639(15) 0.24206(11) 0.0826(14) Uani 1 1 d U U 1 H19E H 0.8414 0.3586 0.2243 0.124 Uiso 1 1 calc R U 1 H19F H 0.8538 0.3208 0.2626 0.124 Uiso 1 1 calc R U 1 H19G H 0.8023 0.3599 0.2613 0.124 Uiso 1 1 calc R U 1 C193 C 0.90101(11) 0.19241(10) 0.87285(9) 0.0445(9) Uani 1 1 d U V 1 H19H H 0.8794 0.1569 0.8530 0.053 Uiso 1 1 calc R V 1 H19I H 0.9322 0.1835 0.8981 0.053 Uiso 1 1 calc R V 1 C194 C 0.92996(13) 0.22270(12) 0.84289(11) 0.0633(11) Uani 1 1 d U V 1 H19J H 0.9519 0.2583 0.8623 0.076 Uiso 1 1 calc R V 1 H19K H 0.8993 0.2310 0.8169 0.076 Uiso 1 1 calc R V 1 C195 C 0.97268(11) 0.18671(12) 0.82239(9) 0.0506(8) Uani 1 1 d U V 1 H19L H 1.0025 0.2112 0.8149 0.061 Uiso 1 1 calc R V 1 H19M H 0.9936 0.1677 0.8466 0.061 Uiso 1 1 calc R V 1 C196 C 0.94262(15) 0.14428(15) 0.77908(12) 0.0401(9) Uiso 0.70 1 d P V 1 H19N H 0.9181 0.1161 0.7873 0.060 Uiso 1 1 calc R V 1 H19O H 0.9722 0.1267 0.7652 0.060 Uiso 1 1 calc R V 1 H19P H 0.9179 0.1622 0.7563 0.060 Uiso 1 1 calc R V 1 C197 C 0.80712(11) 0.23786(11) 0.85808(11) 0.0520(10) Uani 1 1 d U V 1 H19Q H 0.7818 0.2597 0.8747 0.062 Uiso 1 1 calc R V 1 H19R H 0.8234 0.2618 0.8401 0.062 Uiso 1 1 calc R V 1 C198 C 0.76881(12) 0.18920(11) 0.82353(12) 0.0600(11) Uani 1 1 d U V 1 H19S H 0.7521 0.1645 0.8407 0.072 Uiso 1 1 calc R V 1 H19T H 0.7928 0.1678 0.8053 0.072 Uiso 1 1 calc R V 1 C199 C 0.71920(11) 0.20904(13) 0.79017(10) 0.0545(10) Uani 1 1 d U V 1 H19U H 0.6976 0.2331 0.8088 0.065 Uiso 1 1 calc R V 1 H19V H 0.7362 0.2315 0.7715 0.065 Uiso 1 1 calc R V 1 C200 C 0.67653(15) 0.16183(16) 0.75703(12) 0.0926(16) Uani 1 1 d U V 1 H20A H 0.6979 0.1371 0.7393 0.139 Uiso 1 1 calc R V 1 H20B H 0.6469 0.1766 0.7351 0.139 Uiso 1 1 calc R V 1 H20C H 0.6572 0.1411 0.7752 0.139 Uiso 1 1 calc R V 1 C201 C 0.88748(12) 0.27961(10) 0.92454(11) 0.0500(10) Uani 1 1 d U V 1 H20D H 0.8576 0.2988 0.9375 0.060 Uiso 1 1 calc R V 1 H20E H 0.8999 0.3018 0.9036 0.060 Uiso 1 1 calc R V 1 C202 C 0.94058(13) 0.27978(12) 0.96526(11) 0.0652(11) Uani 1 1 d U V 1 H20F H 0.9735 0.2663 0.9528 0.078 Uiso 1 1 calc R V 1 H20G H 0.9305 0.2543 0.9847 0.078 Uiso 1 1 calc R V 1 C203 C 0.96012(13) 0.33879(12) 0.99618(11) 0.0643(11) Uani 1 1 d U V 1 H20H H 0.9981 0.3389 1.0192 0.077 Uiso 1 1 calc R V 1 H20I H 0.9664 0.3647 0.9760 0.077 Uiso 1 1 calc R V 1 C204 C 0.91650(17) 0.35870(18) 1.02191(14) 0.0591(12) Uiso 0.70 1 d P V 1 H20J H 0.8806 0.3637 0.9994 0.089 Uiso 1 1 calc R V 1 H20K H 0.9330 0.3941 1.0437 0.089 Uiso 1 1 calc R V 1 H20L H 0.9072 0.3314 1.0397 0.089 Uiso 1 1 calc R V 1 C205 C 0.83762(11) 0.18700(11) 0.92487(11) 0.0561(10) Uani 1 1 d U V 1 H20M H 0.8725 0.1731 0.9428 0.067 Uiso 1 1 calc R V 1 H20N H 0.8121 0.1545 0.9031 0.067 Uiso 1 1 calc R V 1 C206 C 0.80317(17) 0.21341(18) 0.96042(14) 0.0427(12) Uiso 0.60 1 d P V 1 H20O H 0.8310 0.2360 0.9891 0.051 Uiso 1 1 calc R V 1 H20P H 0.7760 0.2378 0.9461 0.051 Uiso 1 1 calc R V 1 C906 C 0.7756(3) 0.2049(3) 0.9328(2) 0.071(2) Uiso 0.50 1 d P M 2 C207 C 0.76874(15) 0.16704(15) 0.97288(12) 0.0410(9) Uiso 0.70 1 d PD V 1 H20Q H 0.7988 0.1468 0.9897 0.049 Uiso 1 1 calc R V 1 H20R H 0.7497 0.1856 0.9967 0.049 Uiso 1 1 calc R V 1 C208 C 0.7266(2) 0.1268(2) 0.9434(2) 0.0382(16) Uiso 0.40 1 d PD V 1 H20S H 0.6937 0.1442 0.9273 0.057 Uiso 0.40 1 calc PR V 1 H20T H 0.7124 0.1025 0.9616 0.057 Uiso 0.40 1 calc PR V 1 H20U H 0.7434 0.1050 0.9200 0.057 Uiso 0.40 1 calc PR V 1 C209 C 0.53769(9) 0.98046(9) 0.34668(8) 0.0268(6) Uani 1 1 d U W 1 H20V H 0.5350 1.0161 0.3671 0.032 Uiso 1 1 calc R W 1 H20W H 0.5659 0.9878 0.3282 0.032 Uiso 1 1 calc R W 1 C210 C 0.47810(10) 0.96006(11) 0.31303(8) 0.0370(8) Uani 1 1 d U W 1 H21A H 0.4499 0.9504 0.3308 0.044 Uiso 1 1 calc R W 1 H21B H 0.4809 0.9262 0.2904 0.044 Uiso 1 1 calc R W 1 C211 C 0.45576(10) 1.00424(11) 0.28630(10) 0.0461(9) Uani 1 1 d U W 1 H21C H 0.4543 1.0383 0.3092 0.055 Uiso 1 1 calc R W 1 H21D H 0.4839 1.0132 0.2683 0.055 Uiso 1 1 calc R W 1 C212 C 0.39631(12) 0.98679(14) 0.25325(12) 0.0818(13) Uani 1 1 d U W 1 H21E H 0.3975 0.9535 0.2301 0.123 Uiso 1 1 calc R W 1 H21F H 0.3844 1.0166 0.2371 0.123 Uiso 1 1 calc R W 1 H21G H 0.3679 0.9788 0.2709 0.123 Uiso 1 1 calc R W 1 C213 C 0.52654(9) 0.93996(9) 0.41409(7) 0.0277(6) Uani 1 1 d U W 1 H21H H 0.4857 0.9237 0.3973 0.033 Uiso 1 1 calc R W 1 H21I H 0.5252 0.9786 0.4300 0.033 Uiso 1 1 calc R W 1 C214 C 0.55079(10) 0.90688(10) 0.45184(8) 0.0337(7) Uani 1 1 d U W 1 H21J H 0.5437 0.8668 0.4375 0.040 Uiso 1 1 calc R W 1 H21K H 0.5938 0.9174 0.4645 0.040 Uiso 1 1 calc R W 1 C215 C 0.52053(11) 0.91886(12) 0.49172(10) 0.0511(8) Uiso 1 1 d . W 1 H21L H 0.5374 0.8979 0.5158 0.061 Uiso 1 1 calc R W 1 H21M H 0.5299 0.9588 0.5066 0.061 Uiso 1 1 calc R W 1 C216 C 0.45574(14) 0.90495(14) 0.47787(10) 0.0789(12) Uani 1 1 d U W 1 H21N H 0.4376 0.9314 0.4600 0.118 Uiso 1 1 calc R W 1 H21O H 0.4414 0.9068 0.5061 0.118 Uiso 1 1 calc R W 1 H21P H 0.4453 0.8674 0.4583 0.118 Uiso 1 1 calc R W 1 C217 C 0.55824(10) 0.88190(10) 0.35009(8) 0.0336(6) Uiso 1 1 d . W 1 H21Q H 0.5741 0.8583 0.3722 0.040 Uiso 1 1 calc R W 1 H21R H 0.5161 0.8681 0.3357 0.040 Uiso 1 1 calc R W 1 C218 C 0.59020(11) 0.87500(10) 0.31158(9) 0.0408(8) Uani 1 1 d U W 1 H21S H 0.6332 0.8795 0.3258 0.049 Uiso 1 1 calc R W 1 H21T H 0.5814 0.9041 0.2932 0.049 Uiso 1 1 calc R W 1 C219 C 0.57154(12) 0.81823(11) 0.27893(9) 0.0464(9) Uani 1 1 d U W 1 H21U H 0.5292 0.8150 0.2629 0.056 Uiso 1 1 calc R W 1 H21V H 0.5772 0.7893 0.2978 0.056 Uiso 1 1 calc R W 1 C220 C 0.60676(14) 0.80851(13) 0.24204(10) 0.0659(12) Uani 1 1 d U W 1 H22A H 0.6042 0.8390 0.2253 0.099 Uiso 1 1 calc R W 1 H22B H 0.5906 0.7735 0.2196 0.099 Uiso 1 1 calc R W 1 H22C H 0.6480 0.8069 0.2576 0.099 Uiso 1 1 calc R W 1 C221 C 0.62663(10) 0.96256(10) 0.40148(8) 0.0345(7) Uani 1 1 d U W 1 H22D H 0.6464 0.9681 0.3768 0.041 Uiso 1 1 calc R W 1 H22E H 0.6455 0.9339 0.4168 0.041 Uiso 1 1 calc R W 1 C222 C 0.63717(10) 1.01700(10) 0.43837(9) 0.0365(8) Uani 1 1 d U W 1 H22F H 0.6153 1.0452 0.4245 0.044 Uiso 1 1 calc R W 1 H22G H 0.6223 1.0109 0.4654 0.044 Uiso 1 1 calc R W 1 C223 C 0.70193(11) 1.03779(10) 0.45506(11) 0.0486(10) Uani 1 1 d U W 1 H22H H 0.7171 1.0426 0.4278 0.058 Uiso 1 1 calc R W 1 H22I H 0.7236 1.0102 0.4699 0.058 Uiso 1 1 calc R W 1 C224 C 0.71224(13) 1.09261(11) 0.49028(10) 0.0578(11) Uani 1 1 d U W 1 H22J H 0.6922 1.1203 0.4751 0.087 Uiso 1 1 calc R W 1 H22K H 0.7546 1.1050 0.5015 0.087 Uiso 1 1 calc R W 1 H22L H 0.6966 1.0879 0.5170 0.087 Uiso 1 1 calc R W 1 C225 C 0.94173(10) 0.61792(9) 0.65006(8) 0.0291(7) Uani 1 1 d U X 1 H22M H 0.9253 0.6417 0.6282 0.035 Uiso 1 1 calc R X 1 H22N H 0.9839 0.6317 0.6639 0.035 Uiso 1 1 calc R X 1 C226 C 0.91040(10) 0.62405(10) 0.68947(8) 0.0328(8) Uani 1 1 d U X 1 H22O H 0.8673 0.6185 0.6757 0.039 Uiso 1 1 calc R X 1 H22P H 0.9206 0.5954 0.7080 0.039 Uiso 1 1 calc R X 1 C227 C 0.92784(11) 0.68006(10) 0.72094(8) 0.0382(8) Uani 1 1 d U X 1 H22Q H 0.9230 0.7083 0.7014 0.046 Uiso 1 1 calc R X 1 H22R H 0.9700 0.6834 0.7376 0.046 Uiso 1 1 calc R X 1 C228 C 0.89176(14) 0.69236(14) 0.75771(10) 0.0743(12) Uani 1 1 d U X 1 H22S H 0.8497 0.6855 0.7418 0.111 Uiso 1 1 calc R X 1 H22T H 0.9018 0.7312 0.7745 0.111 Uiso 1 1 calc R X 1 H22U H 0.9009 0.6682 0.7802 0.111 Uiso 1 1 calc R X 1 C229 C 0.97212(10) 0.56070(11) 0.58558(8) 0.0358(7) Uiso 1 1 d . X 1 H22V H 1.0129 0.5773 0.6024 0.043 Uiso 1 1 calc R X 1 H22W H 0.9740 0.5221 0.5701 0.043 Uiso 1 1 calc R X 1 C230 C 0.94929(11) 0.59197(11) 0.54791(9) 0.0403(8) Uani 1 1 d U X 1 H23A H 0.9549 0.6321 0.5619 0.048 Uiso 1 1 calc R X 1 H23B H 0.9066 0.5805 0.5343 0.048 Uiso 1 1 calc R X 1 C231 C 0.98135(11) 0.58106(11) 0.50870(8) 0.0484(8) Uani 1 1 d U X 1 H23C H 0.9731 0.5411 0.4938 0.058 Uiso 1 1 calc R X 1 H23D H 0.9643 0.6017 0.4844 0.058 Uiso 1 1 calc R X 1 C232 C 1.04658(12) 0.59639(18) 0.52316(12) 0.1048(16) Uani 1 1 d U X 1 H23E H 1.0559 0.6352 0.5401 0.157 Uiso 1 1 calc R X 1 H23F H 1.0618 0.5915 0.4951 0.157 Uiso 1 1 calc R X 1 H23G H 1.0649 0.5726 0.5437 0.157 Uiso 1 1 calc R X 1 C233 C 0.87227(9) 0.53780(9) 0.59821(8) 0.0295(7) Uani 1 1 d U X 1 H23H H 0.8520 0.5324 0.6227 0.035 Uiso 1 1 calc R X 1 H23I H 0.8538 0.5664 0.5826 0.035 Uiso 1 1 calc R X 1 C234 C 0.86273(10) 0.48406(11) 0.56213(9) 0.0388(8) Uani 1 1 d U X 1 H23J H 0.8851 0.4565 0.5764 0.047 Uiso 1 1 calc R X 1 H23K H 0.8779 0.4904 0.5353 0.047 Uiso 1 1 calc R X 1 C235 C 0.79782(11) 0.46118(11) 0.54430(10) 0.0430(9) Uani 1 1 d U X 1 H23L H 0.7756 0.4883 0.5292 0.052 Uiso 1 1 calc R X 1 H23M H 0.7823 0.4559 0.5713 0.052 Uiso 1 1 calc R X 1 C236 C 0.78828(13) 0.40530(12) 0.50843(11) 0.0622(12) Uani 1 1 d U X 1 H23N H 0.8021 0.4108 0.4811 0.093 Uiso 1 1 calc R X 1 H23O H 0.7463 0.3914 0.4983 0.093 Uiso 1 1 calc R X 1 H23P H 0.8104 0.3784 0.5232 0.093 Uiso 1 1 calc R X 1 C237 C 0.96213(10) 0.52104(10) 0.65306(8) 0.0336(6) Uiso 1 1 d . X 1 H23Q H 0.9647 0.4853 0.6326 0.040 Uiso 1 1 calc R X 1 H23R H 0.9341 0.5136 0.6717 0.040 Uiso 1 1 calc R X 1 C238 C 1.02226(10) 0.54098(10) 0.68689(9) 0.0352(8) Uani 1 1 d U X 1 H23S H 1.0199 0.5745 0.7100 0.042 Uiso 1 1 calc R X 1 H23T H 1.0506 0.5508 0.6693 0.042 Uiso 1 1 calc R X 1 C239 C 1.04352(12) 0.49548(11) 0.71257(9) 0.0433(9) Uani 1 1 d U X 1 H23U H 1.0148 0.4858 0.7299 0.052 Uiso 1 1 calc R X 1 H23V H 1.0452 0.4620 0.6891 0.052 Uiso 1 1 calc R X 1 C240 C 1.10320(15) 0.51237(15) 0.74662(13) 0.0925(15) Uani 1 1 d U X 1 H24A H 1.1325 0.5189 0.7293 0.139 Uiso 1 1 calc R X 1 H24B H 1.1137 0.4828 0.7636 0.139 Uiso 1 1 calc R X 1 H24C H 1.1023 0.5464 0.7692 0.139 Uiso 1 1 calc R X 1 C241 C 0.1719(3) -0.0524(2) 0.73130(17) 0.212(3) Uani 1 1 d U J 1 H24D H 0.1300 -0.0653 0.7171 0.319 Uiso 1 1 calc R J 1 H24E H 0.1946 -0.0841 0.7291 0.319 Uiso 1 1 calc R J 1 H24F H 0.1852 -0.0257 0.7146 0.319 Uiso 1 1 calc R J 1 C242 C 0.18075(16) -0.02497(19) 0.7823(2) 0.172(3) Uani 1 1 d U J 1 H24G H 0.1761 -0.0529 0.8012 0.206 Uiso 1 1 calc R J 1 H24H H 0.2205 -0.0041 0.7953 0.206 Uiso 1 1 calc R J 1 C243 C 0.13594(15) 0.0392(2) 0.82833(12) 0.1192(18) Uani 1 1 d U J 1 H24I H 0.1760 0.0577 0.8451 0.143 Uiso 1 1 calc R J 1 H24J H 0.1254 0.0115 0.8458 0.143 Uiso 1 1 calc R J 1 C244 C 0.09194(16) 0.08221(16) 0.82673(11) 0.0949(16) Uani 1 1 d U J 1 H24K H 0.0885 0.0967 0.7981 0.142 Uiso 1 1 calc R J 1 H24L H 0.1059 0.1127 0.8544 0.142 Uiso 1 1 calc R J 1 H24M H 0.0534 0.0647 0.8268 0.142 Uiso 1 1 calc R J 1 C245 C 0.5801(3) 0.8186(3) 0.9050(2) 0.0644(18) Uiso 0.50 1 d P K 1 H24N H 0.6035 0.8548 0.9188 0.097 Uiso 0.50 1 calc PR K 1 H24O H 0.5572 0.8093 0.9264 0.097 Uiso 0.50 1 calc PR K 1 H24P H 0.5534 0.8199 0.8747 0.097 Uiso 0.50 1 calc PR K 1 C246 C 0.6186(2) 0.7773(2) 0.8980(2) 0.0520(15) Uiso 0.50 1 d P K 1 H24Q H 0.6494 0.7802 0.9276 0.062 Uiso 0.50 1 calc PR K 1 H24R H 0.5958 0.7402 0.8903 0.062 Uiso 0.50 1 calc PR K 1 C247 C 0.6798(3) 0.7379(3) 0.8567(2) 0.081(2) Uiso 0.50 1 d P K 1 H24S H 0.6555 0.7022 0.8405 0.097 Uiso 0.50 1 calc PR K 1 H24T H 0.7060 0.7336 0.8867 0.097 Uiso 0.50 1 calc PR K 1 C248 C 0.7180(3) 0.7613(3) 0.8224(2) 0.0515(19) Uiso 0.40 1 d P K 1 H24U H 0.6955 0.7498 0.7894 0.077 Uiso 0.40 1 calc PR K 1 H24V H 0.7557 0.7460 0.8265 0.077 Uiso 0.40 1 calc PR K 1 H24W H 0.7252 0.8018 0.8312 0.077 Uiso 0.40 1 calc PR K 1 C249 C 0.84891(19) 0.10819(18) 0.39634(15) 0.0625(13) Uiso 0.70 1 d P H 1 H2A9 H 0.8111 0.1039 0.3722 0.075 Uiso 0.70 1 calc PR H 1 H24 H 0.8799 0.1219 0.3826 0.075 Uiso 0.70 1 calc PR H 1 C250 C 0.85979(19) 0.05593(19) 0.40361(16) 0.0696(14) Uiso 0.70 1 d P H 1 H25A H 0.9023 0.0538 0.4109 0.104 Uiso 0.70 1 calc PR H 1 H25B H 0.8402 0.0281 0.3751 0.104 Uiso 0.70 1 calc PR H 1 H25C H 0.8446 0.0488 0.4299 0.104 Uiso 0.70 1 calc PR H 1 C251 C 0.8445(2) 0.2428(2) 0.47816(17) 0.0842(17) Uiso 0.70 1 d P H 1 H25D H 0.8667 0.2311 0.5061 0.126 Uiso 0.70 1 calc PR H 1 H25E H 0.8090 0.2575 0.4844 0.126 Uiso 0.70 1 calc PR H 1 H25F H 0.8689 0.2716 0.4706 0.126 Uiso 0.70 1 calc PR H 1 C252 C 0.8287(2) 0.1982(2) 0.44091(19) 0.0930(18) Uiso 0.70 1 d P H 1 H25G H 0.7855 0.1905 0.4351 0.112 Uiso 0.70 1 calc PR H 1 H25H H 0.8351 0.2132 0.4139 0.112 Uiso 0.70 1 calc PR H 1 C253 C 0.41089(17) 0.41558(18) 0.17306(15) 0.1183(19) Uani 1 1 d U I 1 H25I H 0.4500 0.4337 0.1751 0.177 Uiso 1 1 calc R I 1 H25J H 0.3987 0.3858 0.1448 0.177 Uiso 1 1 calc R I 1 H25K H 0.4123 0.4000 0.2010 0.177 Uiso 1 1 calc R I 1 C254 C 0.36628(16) 0.4584(2) 0.17033(13) 0.148(2) Uani 1 1 d U I 1 H25L H 0.3769 0.4856 0.1525 0.178 Uiso 1 1 calc R I 1 H25M H 0.3264 0.4394 0.1535 0.178 Uiso 1 1 calc R I 1 C255 C 0.32351(14) 0.52337(16) 0.21859(11) 0.0861(12) Uani 1 1 d U I 1 H25N H 0.2839 0.5030 0.2031 0.103 Uiso 1 1 calc R I 1 H25O H 0.3301 0.5523 0.2011 0.103 Uiso 1 1 calc R I 1 C256 C 0.32490(19) 0.5510(2) 0.26830(14) 0.135(2) Uani 1 1 d U I 1 H25P H 0.3133 0.5232 0.2847 0.202 Uiso 1 1 calc R I 1 H25Q H 0.2975 0.5790 0.2677 0.202 Uiso 1 1 calc R I 1 H25R H 0.3648 0.5687 0.2848 0.202 Uiso 1 1 calc R I 1 C257 C 0.10482(11) 0.77547(11) 0.88955(10) 0.0503(9) Uani 1 1 d U Y 1 H257 H 0.0881 0.8065 0.9027 0.060 Uiso 1 1 calc R Y 1 C258 C 0.09332(12) 0.67960(12) 0.85289(12) 0.0784(12) Uani 1 1 d U Y 1 H25S H 0.1355 0.6876 0.8560 0.118 Uiso 1 1 calc R Y 1 H25T H 0.0724 0.6687 0.8195 0.118 Uiso 1 1 calc R Y 1 H25U H 0.0867 0.6494 0.8686 0.118 Uiso 1 1 calc R Y 1 C259 C 0.01088(10) 0.72307(11) 0.87751(10) 0.0470(9) Uani 1 1 d U Y 1 H25V H 0.0020 0.7589 0.8929 0.071 Uiso 1 1 calc R Y 1 H25W H 0.0054 0.6954 0.8960 0.071 Uiso 1 1 calc R Y 1 H25$ H -0.0157 0.7115 0.8459 0.071 Uiso 1 1 calc R Y 1 C260 C 0.65732(12) 1.07037(13) 0.62933(12) 0.0784(12) Uani 1 1 d U Z 1 H26A H 0.6182 1.0608 0.6336 0.118 Uiso 1 1 calc R Z 1 H26B H 0.6537 1.0913 0.6043 0.118 Uiso 1 1 calc R Z 1 H26C H 0.6826 1.0930 0.6588 0.118 Uiso 1 1 calc R Z 1 C261 C 0.74129(11) 1.02852(11) 0.60981(10) 0.0527(9) Uani 1 1 d U Z 1 H26D H 0.7559 0.9925 0.6034 0.079 Uiso 1 1 calc R Z 1 H26E H 0.7676 1.0520 0.6383 0.079 Uiso 1 1 calc R Z 1 H26F H 0.7399 1.0464 0.5831 0.079 Uiso 1 1 calc R Z 1 C262 C 0.65348(11) 0.97234(9) 0.61051(9) 0.0454(8) Uani 1 1 d U Z 1 H262 H 0.6711 0.9407 0.5999 0.055 Uiso 1 1 calc R Z 1 C263 C 0.74628(12) 0.93775(14) 0.33402(11) 0.0635(11) Uani 1 1 d U A 1 H263 H 0.7513 0.9405 0.3668 0.076 Uiso 1 1 calc R A 1 C264 C 0.76657(15) 0.89357(15) 0.26313(10) 0.0774(13) Uani 1 1 d U A 1 H26G H 0.7307 0.8682 0.2469 0.116 Uiso 1 1 calc R A 1 H26H H 0.8005 0.8778 0.2546 0.116 Uiso 1 1 calc R A 1 H26I H 0.7631 0.9293 0.2538 0.116 Uiso 1 1 calc R A 1 C265 C 0.81111(13) 0.86697(12) 0.33917(11) 0.0731(11) Uani 1 1 d U A 1 H26J H 0.8081 0.8742 0.3718 0.110 Uiso 1 1 calc R A 1 H26K H 0.8521 0.8755 0.3388 0.110 Uiso 1 1 calc R A 1 H26L H 0.7977 0.8279 0.3245 0.110 Uiso 1 1 calc R A 1 C266 C 0.48894(11) 0.77701(11) 0.12249(10) 0.0519(10) Uani 1 1 d U B 1 H26M H 0.4984 0.7416 0.1068 0.078 Uiso 1 1 calc R B 1 H26N H 0.5150 0.7882 0.1543 0.078 Uiso 1 1 calc R B 1 H26O H 0.4944 0.8053 0.1046 0.078 Uiso 1 1 calc R B 1 C267 C 0.40615(12) 0.82095(12) 0.14690(14) 0.0874(14) Uani 1 1 d U B 1 H26P H 0.3698 0.8103 0.1552 0.131 Uiso 1 1 calc R B 1 H26Q H 0.3981 0.8455 0.1246 0.131 Uiso 1 1 calc R B 1 H26R H 0.4359 0.8403 0.1754 0.131 Uiso 1 1 calc R B 1 C268 C 0.39339(12) 0.72394(11) 0.10965(10) 0.0524(10) Uani 1 1 d U B 1 H268 H 0.4094 0.6927 0.0960 0.063 Uiso 1 1 calc R B 1 C269 C 0.84665(13) 0.52597(13) 0.38924(10) 0.0549(9) Uiso 1 1 d . C 1 H269 H 0.8286 0.5574 0.3998 0.066 Uiso 1 1 calc R C 1 C270 C 0.84297(12) 0.42887(11) 0.36915(14) 0.0840(14) Uani 1 1 d U C 1 H27A H 0.8375 0.4214 0.3350 0.126 Uiso 1 1 calc R C 1 H27B H 0.8238 0.3975 0.3777 0.126 Uiso 1 1 calc R C 1 H27C H 0.8851 0.4342 0.3849 0.126 Uiso 1 1 calc R C 1 C271 C 0.75854(11) 0.47084(11) 0.39031(10) 0.0492(9) Uani 1 1 d U C 1 H27D H 0.7508 0.5051 0.4091 0.074 Uiso 1 1 calc R C 1 H27E H 0.7556 0.4405 0.4067 0.074 Uiso 1 1 calc R C 1 H27F H 0.7296 0.4619 0.3596 0.074 Uiso 1 1 calc R C 1 C272 C 0.75402(12) 0.56089(12) 0.66532(11) 0.0591(11) Uani 1 1 d U D 1 H272 H 0.7489 0.5575 0.6324 0.071 Uiso 1 1 calc R D 1 C273 C 0.69086(12) 0.63213(13) 0.66135(11) 0.0651(11) Uani 1 1 d U D 1 H27G H 0.7076 0.6709 0.6741 0.098 Uiso 1 1 calc R D 1 H27H H 0.6508 0.6271 0.6651 0.098 Uiso 1 1 calc R D 1 H27I H 0.6898 0.6223 0.6279 0.098 Uiso 1 1 calc R D 1 C274 C 0.73327(15) 0.60691(15) 0.73622(11) 0.0806(14) Uani 1 1 d U D 1 H27J H 0.7634 0.5853 0.7502 0.121 Uiso 1 1 calc R D 1 H27K H 0.6958 0.5955 0.7425 0.121 Uiso 1 1 calc R D 1 H27L H 0.7453 0.6464 0.7501 0.121 Uiso 1 1 calc R D 1 C275 C 0.05903(15) 0.7255(2) 0.63595(16) 0.156(2) Uani 1 1 d U E 1 C276 C 0.0248(3) 0.7592(3) 0.6101(2) 0.0172(15) Uiso 0.30 1 d P E 1 C278 C 0.43892(15) 0.78167(15) 0.36576(12) 0.0772(11) Uiso 1 1 d . F 1 H278 H 0.4714 0.7955 0.3923 0.093 Uiso 1 1 calc R F 1 C279 C 0.3654(3) 0.7195(3) 0.3369(3) 0.035(2) Uiso 0.30 1 d P F 1 H27M H 0.3466 0.7178 0.3625 0.053 Uiso 0.30 1 calc PR F 1 H27N H 0.3549 0.6843 0.3137 0.053 Uiso 0.30 1 calc PR F 1 H27O H 0.3518 0.7497 0.3217 0.053 Uiso 0.30 1 calc PR F 1 C280 C 0.4641(3) 0.6909(3) 0.3723(3) 0.091(3) Uiso 0.50 1 d P F 1 H28A H 0.5052 0.7052 0.3764 0.136 Uiso 0.50 1 calc PR F 1 H28B H 0.4545 0.6553 0.3496 0.136 Uiso 0.50 1 calc PR F 1 H28C H 0.4582 0.6857 0.4025 0.136 Uiso 0.50 1 calc PR F 1 C281 C 0.8822(3) 0.7172(3) 0.3246(2) 0.0691(19) Uiso 0.50 1 d P G 1 C282 C 0.9386(3) 0.7879(3) 0.2751(2) 0.0674(19) Uiso 0.50 1 d P N 1 C293 C 0.8130(3) 0.7571(3) 0.1498(2) 0.069(2) Uiso 0.50 1 d P L 1 C294 C 0.8928(3) 0.7161(3) 0.0946(2) 0.088(2) Uiso 0.60 1 d P L 1 C295 C 0.9241(3) 0.6713(3) 0.0982(2) 0.069(2) Uiso 0.50 1 d P L 1 C297 C 0.6411(2) 0.43932(19) 0.59805(17) 0.0739(15) Uiso 0.70 1 d P M 1 H29A H 0.6495 0.4505 0.5704 0.111 Uiso 0.70 1 calc PR M 1 H29C H 0.6644 0.4651 0.6266 0.111 Uiso 0.70 1 calc PR M 1 H29D H 0.5991 0.4400 0.5963 0.111 Uiso 0.70 1 calc PR M 1 C298 C 0.6557(3) 0.3862(2) 0.5991(2) 0.0766(18) Uiso 0.60 1 d P M 1 H29E H 0.6959 0.3905 0.6201 0.092 Uiso 0.60 1 calc PR M 1 H29F H 0.6291 0.3695 0.6152 0.092 Uiso 0.60 1 calc PR M 1 C299 C 0.66557(19) 0.30207(18) 0.56495(15) 0.0571(12) Uiso 0.70 1 d P M 1 H29G H 0.6334 0.2840 0.5749 0.069 Uiso 0.70 1 calc PR M 1 H29H H 0.7022 0.3040 0.5900 0.069 Uiso 0.70 1 calc PR M 1 C300 C 0.67196(17) 0.26655(17) 0.52357(14) 0.0372(10) Uiso 0.60 1 d P M 1 H30A H 0.6591 0.2838 0.4965 0.056 Uiso 0.60 1 calc PR M 1 H30B H 0.6478 0.2310 0.5182 0.056 Uiso 0.60 1 calc PR M 1 H30C H 0.7133 0.2605 0.5275 0.056 Uiso 0.60 1 calc PR M 1 C080 C 0.4748(2) 0.7415(2) 0.3952(2) 0.0479(15) Uiso 0.50 1 d P O 2 C301 C 0.59777(18) 0.77096(19) 0.68260(15) 0.0427(11) Uiso 0.60 1 d P . . C302 C 0.5727(2) 0.7596(2) 0.72144(17) 0.0508(13) Uiso 0.60 1 d P N . 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 0.03219(9) 0.01444(9) 0.02238(9) 0.00527(7) 0.00777(8) 0.00475(8) Mo2 0.03381(10) 0.01690(9) 0.01870(9) 0.00109(8) 0.00469(8) 0.00024(8) Mo3 0.02963(9) 0.02025(9) 0.01783(9) 0.00537(8) 0.00455(8) 0.00613(8) Mo4 0.02865(10) 0.02038(10) 0.01841(9) 0.00597(8) 0.00487(8) 0.00726(8) Mo5 0.03472(10) 0.01701(10) 0.01758(9) 0.00232(8) 0.00499(8) 0.00013(9) Mo6 0.03281(10) 0.01407(9) 0.02349(10) 0.00486(8) 0.00810(8) 0.00488(8) Mo7 0.02783(9) 0.01431(9) 0.02432(9) 0.00614(7) 0.00850(8) 0.00409(8) Mo8 0.02646(9) 0.01992(9) 0.01849(9) 0.00548(8) 0.00452(8) 0.00489(8) Mo9 0.02849(9) 0.01535(9) 0.01863(9) 0.00048(7) 0.00634(7) 0.00055(8) Mo10 0.02877(10) 0.01421(9) 0.02353(10) 0.00567(8) 0.00877(8) 0.00445(8) Mo11 0.02703(10) 0.02004(10) 0.01929(9) 0.00592(8) 0.00569(8) 0.00432(8) Mo12 0.02690(9) 0.01636(10) 0.01893(9) 0.00082(8) 0.00643(8) 0.00032(8) Mn1 0.0198(2) 0.0145(2) 0.0181(2) 0.00522(17) 0.00681(17) 0.00337(17) Mn2 0.0185(2) 0.0117(2) 0.0135(2) 0.00248(18) 0.00464(17) 0.00350(18) Mn3 0.01842(10) 0.01252(11) 0.01548(10) 0.00309(9) 0.00667(9) 0.00233(9) O1 0.0419(8) 0.0257(8) 0.0299(8) 0.0072(7) 0.0125(7) 0.0057(7) O2 0.0445(9) 0.0237(8) 0.0361(9) 0.0040(7) 0.0112(7) 0.0081(7) O3 0.0262(7) 0.0190(7) 0.0202(7) 0.0029(6) 0.0084(6) 0.0052(6) O4 0.0317(7) 0.0203(8) 0.0259(7) 0.0076(6) 0.0093(6) 0.0028(6) O5 0.0243(7) 0.0241(7) 0.0168(6) 0.0087(6) 0.0092(6) 0.0055(6) O6 0.0379(9) 0.0443(10) 0.0255(8) 0.0053(8) -0.0001(7) -0.0047(8) O7 0.0256(7) 0.0218(7) 0.0187(7) 0.0070(6) 0.0128(5) 0.0060(6) O8 0.0394(8) 0.0173(7) 0.0173(7) 0.0015(6) 0.0057(6) 0.0073(6) O9 0.0266(7) 0.0208(7) 0.0214(7) 0.0045(6) 0.0069(6) 0.0093(6) O10 0.0292(8) 0.0425(10) 0.0320(9) 0.0075(8) -0.0052(7) 0.0065(8) O11 0.0487(9) 0.0274(8) 0.0272(8) 0.0075(7) 0.0103(7) 0.0110(7) O12 0.0643(10) 0.0182(8) 0.0349(9) 0.0063(7) 0.0148(8) 0.0072(8) O13 0.0405(8) 0.0509(10) 0.0445(9) 0.0288(8) 0.0222(7) 0.0188(8) O14 0.0436(9) 0.0260(9) 0.0651(11) 0.0088(8) 0.0242(8) 0.0004(8) O15 0.0292(8) 0.0445(10) 0.0750(11) 0.0244(9) 0.0248(8) 0.0197(7) O16 0.0345(8) 0.0241(8) 0.0243(8) 0.0071(7) 0.0113(7) 0.0053(7) O17 0.0399(9) 0.0254(9) 0.0395(10) 0.0072(8) 0.0019(8) -0.0073(8) O18 0.0248(7) 0.0222(8) 0.0202(7) 0.0036(6) 0.0077(6) 0.0012(6) O19 0.0583(10) 0.0287(9) 0.0240(8) 0.0022(7) 0.0167(7) 0.0081(8) O20 0.0276(7) 0.0190(8) 0.0273(8) 0.0091(6) 0.0127(6) 0.0043(6) O21 0.0299(8) 0.0178(8) 0.0228(8) 0.0049(6) 0.0039(6) -0.0043(7) O22 0.0221(7) 0.0196(8) 0.0241(7) 0.0020(7) 0.0106(6) 0.0024(6) O23 0.0553(9) 0.0214(8) 0.0280(8) 0.0063(7) 0.0188(7) 0.0135(7) O24 0.0420(9) 0.0241(8) 0.0277(8) 0.0101(7) 0.0081(7) 0.0030(7) O25 0.0305(8) 0.0185(8) 0.0255(8) 0.0055(7) 0.0057(7) 0.0092(7) O26 0.0397(9) 0.0418(10) 0.0334(9) 0.0058(8) 0.0063(8) 0.0104(8) O27 0.0502(9) 0.0200(8) 0.0303(8) 0.0116(7) 0.0151(7) 0.0090(7) O28 0.0476(9) 0.0472(10) 0.0564(10) 0.0307(8) 0.0272(8) 0.0270(8) O29 0.0286(9) 0.0313(10) 0.0729(13) 0.0019(10) 0.0101(9) -0.0109(8) O30 0.0638(10) 0.0131(8) 0.0837(12) 0.0158(8) 0.0402(9) 0.0111(8) O31 0.0290(7) 0.0204(8) 0.0223(7) 0.0040(6) 0.0087(6) 0.0040(6) O32 0.0316(8) 0.0269(8) 0.0279(8) 0.0026(7) 0.0060(7) 0.0009(7) O33 0.0417(8) 0.0275(9) 0.0272(8) -0.0006(7) 0.0110(7) 0.0032(7) O34 0.0282(7) 0.0151(7) 0.0249(7) 0.0061(6) 0.0116(6) 0.0025(6) O35 0.0187(6) 0.0190(7) 0.0208(7) 0.0020(6) 0.0133(5) 0.0011(6) O36 0.0380(8) 0.0215(8) 0.0322(8) 0.0050(7) 0.0157(7) 0.0075(7) O37 0.0382(8) 0.0280(8) 0.0276(8) 0.0142(7) 0.0116(7) 0.0054(7) O38 0.0254(7) 0.0273(8) 0.0286(8) 0.0094(7) 0.0087(6) 0.0002(7) O39 0.0337(8) 0.0298(9) 0.0356(8) 0.0104(7) 0.0105(7) 0.0064(7) O40 0.0335(8) 0.0294(9) 0.0335(8) 0.0102(7) 0.0054(7) 0.0016(7) O41 0.0315(8) 0.0219(8) 0.0123(7) 0.0026(6) 0.0058(6) 0.0017(7) O42 0.0200(7) 0.0202(7) 0.0227(7) 0.0035(6) 0.0061(6) 0.0009(6) O43 0.0177(6) 0.0210(7) 0.0140(6) 0.0038(6) 0.0105(5) 0.0080(6) O44 0.0232(7) 0.0151(7) 0.0189(7) 0.0033(6) 0.0020(6) -0.0033(6) O45 0.0254(7) 0.0167(7) 0.0186(7) 0.0022(6) 0.0125(6) 0.0054(6) O46 0.0213(7) 0.0217(8) 0.0193(7) 0.0109(6) 0.0055(6) 0.0058(6) O47 0.0482(9) 0.0183(8) 0.0238(8) -0.0017(7) 0.0099(7) 0.0040(7) O48 0.0287(8) 0.0316(9) 0.0232(8) -0.0021(7) 0.0039(7) -0.0020(7) O49 0.0437(9) 0.0200(8) 0.0392(9) 0.0049(7) 0.0139(8) 0.0092(7) O50 0.0339(8) 0.0317(9) 0.0284(8) 0.0093(7) 0.0090(7) 0.0013(7) O51 0.0321(8) 0.0180(8) 0.0254(8) 0.0008(7) 0.0065(7) -0.0009(7) O52 0.0306(7) 0.0140(7) 0.0253(8) 0.0062(6) 0.0086(6) 0.0137(6) O53 0.0334(9) 0.0342(9) 0.0313(9) 0.0111(8) 0.0022(7) 0.0083(8) O54 0.0449(9) 0.0328(9) 0.0171(7) 0.0113(7) 0.0093(7) 0.0037(8) O55 0.0320(7) 0.0507(10) 0.0459(9) 0.0201(8) 0.0233(7) 0.0176(7) O56 0.0259(8) 0.0346(10) 0.0711(11) 0.0098(9) 0.0202(8) -0.0043(7) O57 0.0427(8) 0.0213(8) 0.0620(10) 0.0168(7) 0.0308(7) 0.0073(7) O58 0.0382(8) 0.0304(8) 0.0420(8) 0.0259(7) 0.0224(7) 0.0139(7) O59 0.0427(9) 0.0108(8) 0.0506(10) 0.0003(8) 0.0149(8) -0.0037(7) O60 0.0512(9) 0.0244(9) 0.0540(10) 0.0112(8) 0.0301(8) 0.0169(8) O61 0.0731(11) 0.0360(12) 0.1217(16) -0.0031(12) 0.0561(11) -0.0084(10) O62 0.0607(10) 0.0343(10) 0.0778(12) 0.0021(10) 0.0410(9) -0.0121(9) O63 0.0820(15) 0.0873(17) 0.0873(16) 0.0334(14) 0.0195(13) 0.0216(13) O64 0.0602(11) 0.0356(12) 0.1353(18) -0.0081(12) 0.0515(11) -0.0213(10) O65 0.0659(11) 0.0367(12) 0.0917(14) 0.0033(11) 0.0392(11) -0.0164(10) O66 0.0750(13) 0.0610(13) 0.1102(17) 0.0399(12) 0.0332(12) 0.0338(11) O70 0.167(2) 0.1215(19) 0.0570(14) 0.0266(14) 0.0395(14) 0.0879(16) O71 0.0657(12) 0.1180(19) 0.154(2) 0.0440(17) 0.0426(14) 0.0593(12) O72 0.0979(17) 0.144(2) 0.0298(11) 0.0178(14) -0.0077(12) -0.0222(17) O73 0.098(3) 0.093(3) 0.033(2) 0.011(2) -0.014(2) 0.034(3) O74 0.076(3) 0.093(4) 0.067(3) -0.019(3) -0.032(3) 0.034(3) N1 0.0205(8) 0.0353(10) 0.0276(9) 0.0117(8) 0.0127(7) 0.0110(8) N2 0.0268(9) 0.0319(11) 0.0231(9) 0.0115(8) 0.0147(7) 0.0046(8) N3 0.0328(9) 0.0230(9) 0.0203(8) 0.0090(7) 0.0119(7) 0.0089(8) N4 0.0161(8) 0.0251(10) 0.0287(9) 0.0080(8) 0.0174(7) 0.0028(7) N5 0.0627(12) 0.0270(11) 0.0268(10) -0.0055(9) 0.0171(9) 0.0071(10) N6 0.0492(13) 0.0512(14) 0.0201(10) 0.0067(10) -0.0038(10) 0.0111(11) N7 0.0470(11) 0.0349(10) 0.0736(14) 0.0327(10) 0.0212(10) 0.0315(9) N8 0.0454(12) 0.0237(12) 0.0842(17) 0.0019(12) 0.0212(12) 0.0025(10) N9 0.0230(9) 0.0176(9) 0.0391(11) 0.0021(8) 0.0061(8) 0.0046(8) N10 0.0385(10) 0.0308(10) 0.0268(9) 0.0177(8) 0.0189(8) 0.0111(9) N11 0.0391(10) 0.0188(10) 0.0635(13) -0.0042(10) 0.0209(10) -0.0147(9) N12 0.0387(10) 0.0210(10) 0.0454(11) 0.0042(9) 0.0197(9) 0.0110(8) N13 0.0542(12) 0.0593(15) 0.0668(14) 0.0272(12) 0.0306(11) 0.0170(12) N14 0.0463(11) 0.0343(12) 0.0544(13) 0.0044(11) 0.0311(10) 0.0051(10) N15 0.0418(11) 0.0267(11) 0.0519(13) 0.0003(10) 0.0185(10) -0.0172(10) N16 0.0551(13) 0.0558(14) 0.0487(13) 0.0270(11) 0.0140(11) 0.0153(12) C1 0.0224(9) 0.0213(10) 0.0475(12) 0.0226(9) 0.0178(9) 0.0129(8) C2 0.0233(10) 0.0479(15) 0.0334(12) 0.0087(11) 0.0155(9) 0.0040(10) C3 0.0313(11) 0.0196(11) 0.0316(11) 0.0059(10) 0.0123(9) 0.0043(9) C4 0.0199(9) 0.0297(12) 0.0165(10) -0.0006(9) 0.0100(8) 0.0002(9) C6 0.0246(10) 0.0187(11) 0.0345(12) 0.0070(10) 0.0067(9) 0.0038(9) C8 0.0363(11) 0.0265(12) 0.0202(10) 0.0015(9) 0.0111(9) 0.0110(10) C9 0.0225(9) 0.0238(11) 0.0292(10) 0.0059(9) 0.0185(8) -0.0049(9) C10 0.0142(9) 0.0267(12) 0.0381(12) 0.0034(10) 0.0149(8) 0.0031(9) C11 0.0237(10) 0.0157(10) 0.0343(12) 0.0026(9) 0.0057(9) 0.0083(8) C12 0.0157(9) 0.0404(14) 0.0365(12) 0.0038(11) 0.0131(9) -0.0017(10) C13 0.0302(11) 0.0174(11) 0.0429(13) -0.0040(10) 0.0193(10) -0.0007(9) C14 0.0449(13) 0.0326(14) 0.0452(14) -0.0056(12) 0.0182(12) 0.0054(12) C15 0.0553(14) 0.0302(15) 0.084(2) -0.0098(14) 0.0343(14) 0.0114(12) C19 0.0326(11) 0.0057(9) 0.0471(13) 0.0028(9) 0.0190(10) 0.0041(9) C20 0.0299(11) 0.0239(12) 0.0528(15) -0.0027(12) 0.0121(11) 0.0126(10) C23 0.0757(17) 0.0145(12) 0.0580(16) -0.0092(12) 0.0301(14) -0.0037(12) C25 0.0285(11) 0.0205(12) 0.0397(13) -0.0048(11) 0.0084(10) 0.0027(10) C26 0.0499(15) 0.0301(13) 0.0370(14) 0.0106(11) 0.0035(12) 0.0008(12) C27 0.1022(17) 0.0168(12) 0.0431(12) 0.0000(10) 0.0535(11) -0.0053(13) C28 0.0682(14) 0.0325(15) 0.104(2) -0.0188(15) 0.0633(13) -0.0246(13) C29 0.0565(16) 0.0483(18) 0.0698(19) -0.0120(16) 0.0276(14) -0.0140(15) C30 0.0450(12) 0.0403(15) 0.0347(12) -0.0098(11) 0.0306(9) -0.0101(12) C38 0.0283(11) 0.0261(12) 0.0173(10) -0.0017(10) 0.0118(9) -0.0030(10) C39 0.0247(10) 0.0315(12) 0.0190(10) 0.0117(9) 0.0145(8) 0.0126(9) C40 0.0225(10) 0.0185(11) 0.0362(12) 0.0150(9) 0.0149(9) 0.0127(9) C41 0.0320(11) 0.0172(11) 0.0340(12) 0.0032(9) 0.0177(9) 0.0082(9) C42 0.0232(10) 0.0253(12) 0.0303(11) 0.0056(10) 0.0170(9) 0.0108(9) C43 0.0186(10) 0.0129(10) 0.0344(12) 0.0001(9) 0.0060(9) 0.0048(8) C44 0.0177(10) 0.0143(11) 0.0329(12) 0.0032(10) 0.0053(9) -0.0052(9) C45 0.0301(11) 0.0233(12) 0.0306(13) 0.0009(10) 0.0041(10) 0.0151(10) C46 0.0333(12) 0.0166(11) 0.0256(11) 0.0068(9) 0.0039(10) 0.0064(10) C48 0.0541(13) 0.0050(10) 0.0514(14) 0.0082(10) 0.0340(11) 0.0122(10) C49 0.0287(12) 0.0238(13) 0.0520(15) 0.0064(12) 0.0148(11) 0.0009(10) C53 0.0741(17) 0.109(3) 0.0303(13) -0.0156(16) 0.0342(12) -0.0443(18) C54 0.0416(13) 0.0440(16) 0.0398(14) -0.0044(13) 0.0251(11) -0.0140(12) C55 0.0531(13) 0.0195(12) 0.0468(14) 0.0061(11) 0.0274(11) 0.0106(10) C56 0.0681(15) 0.0551(14) 0.0878(16) 0.0592(12) 0.0495(13) 0.0397(12) C59 0.0416(13) 0.0296(14) 0.0419(14) -0.0019(12) 0.0156(12) -0.0124(12) C60 0.0237(10) 0.0360(14) 0.0370(13) 0.0060(11) 0.0192(9) 0.0040(10) C61 0.0476(12) 0.0205(12) 0.0402(12) 0.0063(10) 0.0344(10) 0.0091(10) C62 0.0590(13) 0.0220(13) 0.0408(12) 0.0023(10) 0.0402(10) 0.0063(11) C63 0.0579(16) 0.0400(17) 0.0508(17) 0.0020(14) 0.0164(14) 0.0013(14) C64 0.1021(19) 0.0436(16) 0.0491(13) 0.0191(12) 0.0586(12) 0.0101(15) C65 0.0477(14) 0.0435(17) 0.090(2) 0.0075(16) 0.0433(13) -0.0135(13) C66 0.0263(12) 0.0372(15) 0.0615(18) 0.0043(14) 0.0096(12) -0.0065(12) C68 0.0422(10) 0.0155(11) 0.0827(15) 0.0123(11) 0.0500(10) 0.0126(9) C72 0.0871(17) 0.0152(12) 0.0443(14) -0.0033(11) 0.0343(13) 0.0123(12) C73 0.0125(9) 0.0276(12) 0.0336(11) 0.0046(10) 0.0120(8) 0.0020(9) C74 0.0270(10) 0.0295(12) 0.0203(10) 0.0093(9) 0.0131(8) -0.0009(9) C76 0.0293(9) 0.0186(10) 0.0213(9) 0.0032(8) 0.0214(8) 0.0066(8) C77 0.0316(10) 0.0045(9) 0.0337(11) -0.0008(8) 0.0206(8) 0.0007(8) C78 0.0281(10) 0.0322(12) 0.0248(11) -0.0023(10) 0.0169(8) 0.0183(9) C80 0.0214(10) 0.0199(10) 0.0235(10) 0.0093(9) 0.0082(8) 0.0008(9) C81 0.0308(11) 0.0279(12) 0.0235(10) 0.0125(9) 0.0082(9) 0.0093(10) C83 0.0291(10) 0.0044(9) 0.0400(12) 0.0054(9) 0.0095(10) 0.0028(8) C84 0.0207(9) 0.0299(13) 0.0387(12) -0.0053(11) 0.0202(9) -0.0042(10) C85 0.0202(10) 0.0225(11) 0.0585(14) 0.0229(10) 0.0159(10) 0.0053(9) C86 0.0543(14) 0.0450(17) 0.0591(16) -0.0150(14) 0.0361(12) -0.0111(13) C90 0.0502(14) 0.0134(11) 0.0468(14) 0.0037(11) 0.0177(12) -0.0037(11) C91 0.0245(10) 0.0190(11) 0.0290(11) -0.0015(9) 0.0082(9) 0.0069(9) C92 0.0389(12) 0.0320(13) 0.0458(14) 0.0089(12) 0.0157(11) 0.0147(11) C93 0.0519(12) 0.0229(11) 0.0774(15) 0.0284(11) 0.0480(10) 0.0183(10) C94 0.0458(13) 0.0091(11) 0.0704(17) -0.0083(12) 0.0271(12) -0.0046(10) C95 0.0416(13) 0.0427(15) 0.0533(15) 0.0110(13) 0.0230(11) 0.0160(12) C96 0.0251(10) 0.0215(11) 0.0509(13) 0.0139(10) 0.0185(10) 0.0013(9) C97 0.0144(9) 0.0125(10) 0.0477(14) 0.0038(10) 0.0053(9) 0.0023(8) C98 0.0478(12) 0.0294(13) 0.0211(10) 0.0051(10) 0.0207(9) 0.0043(11) C99 0.0727(14) 0.0380(15) 0.0375(11) 0.0008(11) 0.0456(10) -0.0029(13) C100 0.0517(11) 0.0278(13) 0.0892(16) 0.0122(12) 0.0583(10) 0.0007(11) C101 0.0405(12) 0.0362(14) 0.0500(14) 0.0135(12) 0.0265(11) 0.0040(11) C102 0.0562(12) 0.0228(11) 0.0345(11) 0.0154(9) 0.0334(9) 0.0173(10) C103 0.0408(10) 0.0169(10) 0.0371(11) 0.0094(9) 0.0330(8) 0.0105(9) C104 0.0529(13) 0.0217(13) 0.0445(14) -0.0118(11) 0.0261(11) -0.0099(11) C105 0.0820(18) 0.0468(18) 0.0674(17) -0.0024(15) 0.0475(14) -0.0055(16) C106 0.1098(16) 0.0251(14) 0.0826(15) -0.0014(12) 0.0833(12) 0.0147(13) C109 0.0244(10) 0.0175(11) 0.0310(12) 0.0081(9) 0.0125(9) 0.0101(9) C111 0.0212(10) 0.0270(12) 0.0176(10) 0.0042(9) 0.0065(9) 0.0010(10) C112 0.0250(9) 0.0239(11) 0.0291(10) 0.0100(9) 0.0238(8) 0.0062(8) C114 0.0222(10) 0.0362(13) 0.0215(10) 0.0088(10) 0.0152(8) 0.0070(10) C115 0.0242(10) 0.0124(10) 0.0381(12) 0.0083(9) 0.0107(9) 0.0033(8) C116 0.0256(10) 0.0164(11) 0.0255(11) 0.0001(9) 0.0101(9) 0.0058(9) C117 0.0261(11) 0.0216(12) 0.0257(12) 0.0011(10) 0.0076(9) 0.0079(10) C118 0.0257(10) 0.0108(9) 0.0263(10) 0.0082(8) 0.0119(8) 0.0041(8) C119 0.0254(11) 0.0112(10) 0.0382(12) 0.0145(9) 0.0071(10) -0.0061(9) C120 0.0300(11) 0.0162(12) 0.0398(12) -0.0121(10) 0.0248(9) -0.0020(9) C121 0.0352(12) 0.0366(15) 0.0497(14) -0.0125(13) 0.0293(10) -0.0009(11) C125 0.0394(12) 0.0268(11) 0.0695(16) 0.0305(11) 0.0223(12) 0.0261(10) C126 0.0252(10) 0.0162(11) 0.0518(14) 0.0079(11) 0.0216(10) 0.0012(9) C127 0.0339(11) 0.0275(12) 0.0395(12) 0.0198(10) 0.0214(10) 0.0037(10) C128 0.0516(15) 0.0376(16) 0.0464(15) 0.0111(13) 0.0180(13) 0.0085(13) C129 0.0418(13) 0.0439(15) 0.0740(17) 0.0317(13) 0.0335(12) 0.0130(12) C130 0.0241(11) 0.0160(12) 0.0622(17) -0.0110(12) 0.0096(12) -0.0036(10) C131 0.0298(12) 0.0264(13) 0.0410(14) -0.0069(12) 0.0068(11) 0.0091(10) C132 0.0399(11) 0.0170(11) 0.0190(10) 0.0054(9) 0.0204(9) 0.0064(10) C133 0.0218(10) 0.0294(13) 0.0497(15) 0.0075(12) 0.0171(10) -0.0003(10) C136 0.0158(11) 0.0430(16) 0.0572(17) 0.0069(14) 0.0049(11) -0.0031(11) C137 0.0113(10) 0.0369(14) 0.0402(14) 0.0007(12) -0.0070(10) -0.0081(10) C138 0.0437(14) 0.0442(16) 0.0540(16) 0.0151(13) 0.0245(12) 0.0025(13) C139 0.129(2) 0.0212(15) 0.0575(14) -0.0143(12) 0.0708(14) -0.0163(15) C140 0.0605(14) 0.0421(14) 0.143(2) 0.0610(14) 0.0634(15) 0.0375(12) C143 0.0349(12) 0.0224(12) 0.0348(13) 0.0069(11) 0.0144(10) -0.0012(10) C144 0.0482(12) 0.0145(10) 0.0293(11) 0.0150(9) 0.0262(9) 0.0128(10) C145 0.0544(14) 0.0378(15) 0.0227(12) -0.0004(11) 0.0137(11) 0.0031(12) C146 0.0563(15) 0.0394(15) 0.0369(14) 0.0048(12) 0.0146(12) 0.0186(12) C147 0.0618(15) 0.0621(17) 0.0325(12) 0.0185(12) 0.0250(11) 0.0244(14) C148 0.0653(18) 0.075(2) 0.0776(19) 0.0456(16) 0.0226(16) 0.0195(17) C149 0.0397(14) 0.0508(15) 0.0290(12) 0.0183(12) -0.0102(11) 0.0068(12) C150 0.102(2) 0.0501(17) 0.0550(18) -0.0050(15) 0.0285(16) 0.0384(16) C151 0.080(2) 0.102(2) 0.0559(19) 0.0341(18) -0.0041(18) 0.0373(19) C153 0.0531(14) 0.0344(14) 0.0337(13) 0.0070(11) 0.0148(11) 0.0122(12) C154 0.082(2) 0.0463(17) 0.0259(13) -0.0061(13) 0.0082(14) -0.0141(16) C157 0.0531(15) 0.0463(16) 0.0213(12) -0.0023(12) 0.0049(11) 0.0046(13) C158 0.0550(16) 0.075(2) 0.0448(17) 0.0026(16) 0.0073(14) 0.0280(15) C159 0.088(2) 0.082(2) 0.068(2) 0.0010(19) 0.0355(17) 0.0383(18) C161 0.0537(15) 0.0341(15) 0.0320(13) -0.0042(12) 0.0168(12) 0.0104(12) C162 0.081(2) 0.071(2) 0.0339(16) -0.0112(16) 0.0099(15) 0.0324(17) C163 0.065(2) 0.099(3) 0.0463(19) -0.008(2) 0.0102(16) 0.014(2) C165 0.0466(14) 0.0430(15) 0.0249(13) 0.0053(12) 0.0038(12) 0.0163(12) C166 0.0479(15) 0.069(2) 0.0300(14) 0.0105(14) 0.0126(12) -0.0022(15) C167 0.0541(17) 0.0542(19) 0.063(2) 0.0135(17) 0.0058(16) 0.0085(16) C168 0.075(2) 0.092(3) 0.082(2) 0.035(2) 0.0284(18) 0.003(2) C169 0.0602(18) 0.0489(18) 0.0255(14) -0.0047(14) -0.0030(13) -0.0073(15) C170 0.0747(19) 0.0584(19) 0.0384(15) 0.0174(14) 0.0137(15) 0.0171(16) C171 0.198(3) 0.065(2) 0.0463(16) -0.0110(16) 0.0632(18) -0.056(2) C173 0.0729(17) 0.0464(17) 0.0374(15) -0.0036(14) 0.0226(13) 0.0218(14) C174 0.0631(19) 0.075(2) 0.0443(17) 0.0172(16) -0.0066(16) 0.0237(17) C175 0.0700(18) 0.078(2) 0.092(2) 0.022(2) 0.0308(18) 0.0423(17) C176 0.109(2) 0.120(2) 0.106(3) 0.022(2) 0.014(2) 0.0999(16) C177 0.0611(16) 0.0287(14) 0.0646(18) 0.0098(14) 0.0165(15) 0.0089(13) C178 0.0606(17) 0.0379(16) 0.084(2) 0.0079(16) 0.0052(17) 0.0233(14) C179 0.064(2) 0.084(3) 0.083(3) -0.012(2) -0.007(2) 0.014(2) C180 0.179(5) 0.136(4) 0.125(4) -0.039(4) 0.007(4) 0.042(4) C181 0.0648(17) 0.0355(15) 0.094(2) 0.0225(15) 0.0332(16) 0.0201(13) C182 0.144(3) 0.101(3) 0.189(4) 0.074(3) 0.107(2) 0.080(2) C185 0.0447(14) 0.0368(15) 0.088(2) 0.0210(15) 0.0255(14) 0.0118(12) C186 0.0696(17) 0.0489(17) 0.090(2) 0.0293(16) 0.0365(16) 0.0179(15) C187 0.070(2) 0.058(2) 0.240(5) -0.057(3) -0.046(3) 0.0309(19) C188 0.199(5) 0.139(3) 0.251(5) 0.128(3) 0.106(4) 0.081(3) C189 0.0539(16) 0.0246(14) 0.076(2) 0.0014(14) 0.0092(15) 0.0129(12) C190 0.0621(17) 0.061(2) 0.089(2) 0.0117(19) 0.0286(17) 0.0166(16) C191 0.0654(18) 0.063(2) 0.0454(16) -0.0040(16) 0.0194(14) -0.0015(16) C192 0.087(2) 0.097(3) 0.068(2) 0.006(2) 0.0413(17) 0.000(2) C193 0.0481(14) 0.0332(13) 0.0617(17) 0.0214(13) 0.0173(13) 0.0279(11) C194 0.090(2) 0.0517(18) 0.0653(18) 0.0237(15) 0.0361(16) 0.0326(16) C195 0.0539(13) 0.0606(17) 0.0661(14) 0.0402(12) 0.0451(11) 0.0212(13) C197 0.0433(14) 0.0450(16) 0.0735(19) 0.0235(15) 0.0121(14) 0.0257(12) C198 0.0520(17) 0.0215(14) 0.091(2) -0.0022(16) -0.0015(17) 0.0077(13) C199 0.0402(14) 0.066(2) 0.0628(18) 0.0187(16) 0.0217(13) -0.0006(15) C200 0.087(2) 0.111(3) 0.059(2) -0.001(2) 0.009(2) -0.034(2) C201 0.0492(15) 0.0261(13) 0.075(2) 0.0202(13) 0.0037(15) 0.0207(12) C202 0.0668(19) 0.0648(19) 0.079(2) 0.0453(16) 0.0189(16) 0.0269(16) C203 0.0643(19) 0.0480(17) 0.073(2) 0.0237(16) -0.0087(17) 0.0206(15) C205 0.0506(15) 0.0401(16) 0.094(2) 0.0281(15) 0.0337(15) 0.0233(13) C209 0.0318(10) 0.0222(10) 0.0382(11) 0.0229(9) 0.0149(9) 0.0172(9) C210 0.0393(13) 0.0462(15) 0.0268(12) 0.0121(11) 0.0083(10) 0.0036(12) C211 0.0378(13) 0.0541(15) 0.0576(15) 0.0299(13) 0.0149(12) 0.0223(12) C212 0.0449(17) 0.083(2) 0.115(3) 0.0574(19) -0.0122(18) 0.0116(17) C213 0.0279(9) 0.0341(12) 0.0373(11) 0.0206(9) 0.0248(8) 0.0195(9) C214 0.0410(12) 0.0345(13) 0.0359(12) 0.0164(10) 0.0220(10) 0.0068(11) C216 0.120(2) 0.084(2) 0.0565(16) 0.0327(16) 0.0492(16) 0.030(2) C218 0.0464(13) 0.0343(14) 0.0506(14) 0.0172(12) 0.0219(11) 0.0080(12) C219 0.0729(17) 0.0312(14) 0.0333(13) 0.0018(12) 0.0141(13) 0.0062(14) C220 0.097(2) 0.0530(19) 0.0439(17) 0.0117(15) 0.0062(17) 0.0203(18) C221 0.0375(12) 0.0350(13) 0.0391(12) 0.0154(11) 0.0173(10) 0.0123(11) C222 0.0379(13) 0.0312(13) 0.0410(14) 0.0085(11) 0.0098(11) 0.0081(11) C223 0.0431(14) 0.0225(13) 0.0713(19) 0.0049(14) 0.0024(14) 0.0025(12) C224 0.0556(17) 0.0363(15) 0.067(2) 0.0138(15) -0.0141(16) 0.0037(14) C225 0.0452(12) 0.0139(10) 0.0364(12) 0.0120(9) 0.0186(10) 0.0121(9) C226 0.0445(13) 0.0279(13) 0.0278(12) 0.0007(11) 0.0157(11) 0.0097(11) C227 0.0544(15) 0.0364(14) 0.0276(12) 0.0144(11) 0.0076(12) 0.0210(12) C228 0.106(2) 0.071(2) 0.0582(18) -0.0011(17) 0.0487(16) 0.0365(18) C230 0.0458(14) 0.0410(15) 0.0431(14) 0.0212(12) 0.0157(12) 0.0169(12) C231 0.0820(16) 0.0463(15) 0.0405(12) 0.0261(11) 0.0415(11) 0.0296(13) C232 0.0607(16) 0.192(4) 0.106(2) 0.077(2) 0.0643(15) 0.042(2) C233 0.0257(11) 0.0245(12) 0.0392(13) 0.0052(11) 0.0107(10) 0.0056(10) C234 0.0352(13) 0.0406(15) 0.0412(15) 0.0038(13) 0.0130(11) 0.0106(12) C235 0.0417(15) 0.0371(15) 0.0474(16) 0.0137(13) 0.0026(13) 0.0041(13) C236 0.0620(19) 0.0336(17) 0.080(2) -0.0016(17) 0.0065(18) 0.0074(15) C238 0.0336(13) 0.0294(13) 0.0479(14) 0.0211(11) 0.0101(11) 0.0052(11) C239 0.0519(16) 0.0336(15) 0.0381(15) 0.0103(12) -0.0024(13) 0.0059(13) C240 0.084(3) 0.082(2) 0.098(3) 0.054(2) -0.024(2) -0.014(2) C241 0.248(6) 0.148(5) 0.142(4) 0.022(4) -0.126(4) 0.007(5) C242 0.042(2) 0.123(3) 0.351(7) 0.110(4) 0.001(3) 0.027(2) C243 0.080(2) 0.216(4) 0.042(2) -0.012(3) -0.0074(18) 0.078(2) C244 0.111(3) 0.108(3) 0.0439(19) 0.010(2) -0.004(2) -0.028(3) C253 0.103(3) 0.158(4) 0.116(3) 0.072(3) 0.028(3) 0.055(3) C254 0.074(2) 0.264(5) 0.062(2) -0.070(3) 0.004(2) 0.060(3) C255 0.0966(19) 0.125(3) 0.0817(18) 0.0643(18) 0.0627(15) 0.0609(19) C256 0.147(3) 0.179(5) 0.092(3) 0.019(3) 0.052(3) 0.062(3) C257 0.0500(13) 0.0345(15) 0.0751(17) 0.0021(14) 0.0395(12) 0.0080(12) C258 0.0768(17) 0.0335(17) 0.133(3) -0.0115(18) 0.0674(16) -0.0011(15) C259 0.0280(12) 0.0439(16) 0.0598(17) -0.0074(14) 0.0116(12) -0.0084(12) C260 0.0625(15) 0.061(2) 0.141(2) 0.0413(18) 0.0653(15) 0.0070(15) C261 0.0557(15) 0.0314(15) 0.0759(18) 0.0017(14) 0.0350(13) -0.0001(13) C262 0.0646(13) 0.0075(11) 0.0700(15) -0.0127(11) 0.0495(11) -0.0130(10) C263 0.0374(15) 0.101(2) 0.0527(17) 0.0356(17) -0.0003(14) -0.0003(17) C264 0.109(2) 0.080(2) 0.0512(17) 0.0152(17) 0.0358(17) 0.014(2) C265 0.0608(17) 0.0901(19) 0.101(2) 0.0739(15) 0.0324(15) 0.0383(15) C266 0.0576(16) 0.0388(16) 0.0637(18) 0.0074(15) 0.0236(14) 0.0183(13) C267 0.0557(15) 0.0371(19) 0.176(3) -0.006(2) 0.0689(17) -0.0109(15) C268 0.0666(17) 0.0238(15) 0.0627(18) -0.0074(14) 0.0283(15) -0.0170(14) C270 0.0617(16) 0.0182(15) 0.180(3) -0.0001(19) 0.0633(19) 0.0053(13) C271 0.0481(14) 0.0294(15) 0.0756(19) 0.0040(14) 0.0325(13) 0.0024(13) C272 0.0677(17) 0.0505(18) 0.0711(19) 0.0150(16) 0.0354(15) 0.0215(15) C273 0.0445(15) 0.080(2) 0.082(2) 0.0363(18) 0.0243(15) 0.0013(16) C274 0.089(2) 0.090(3) 0.059(2) 0.012(2) 0.0100(19) 0.028(2) C275 0.0468(19) 0.249(6) 0.119(3) -0.073(4) 0.028(2) -0.042(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.7176(17) . ? Mo1 O2 1.7188(16) . ? Mo1 O4 1.9120(14) . ? Mo1 O9 1.9241(12) . ? Mo1 O3 2.3412(14) . ? Mo1 O5 2.3875(15) . ? Mo2 O6 1.6997(15) . ? Mo2 O12 1.7135(17) . ? Mo2 O4 1.9307(16) . ? Mo2 O8 1.9313(15) . ? Mo2 O5 2.3723(12) . ? Mo2 O7 2.3728(13) . ? Mo3 O11 1.6938(17) . ? Mo3 O10 1.7119(15) . ? Mo3 O8 1.9200(15) 2_575 ? Mo3 O9 1.9207(13) . ? Mo3 O3 2.3471(12) . ? Mo3 O7 2.3948(15) 2_575 ? Mo4 O26 1.6954(16) . ? Mo4 O27 1.7121(17) . ? Mo4 O25 1.9163(14) . ? Mo4 O16 1.9319(15) . ? Mo4 O22 2.3532(13) . ? Mo4 O18 2.3854(16) . ? Mo5 O17 1.6998(15) . ? Mo5 O19 1.7112(17) . ? Mo5 O16 1.9147(16) . ? Mo5 O21 1.9181(16) . ? Mo5 O18 2.3673(14) . ? Mo5 O20 2.3707(13) . ? Mo6 O24 1.7061(17) . ? Mo6 O23 1.7102(16) . ? Mo6 O21 1.9139(14) 2_665 ? Mo6 O25 1.9193(13) . ? Mo6 O22 2.3481(14) . ? Mo6 O20 2.3866(16) 2_665 ? Mo7 O49 1.7057(16) . ? Mo7 O50 1.7127(17) . ? Mo7 O51 1.9214(14) . ? Mo7 O52 1.9251(13) . ? Mo7 O46 2.3442(15) . ? Mo7 O45 2.4044(14) . ? Mo8 O54 1.7008(17) . ? Mo8 O53 1.7165(15) . ? Mo8 O31 1.9200(15) . ? Mo8 O52 1.9233(14) . ? Mo8 O45 2.3393(12) . ? Mo8 O43 2.3903(14) . ? Mo9 O33 1.7048(16) . ? Mo9 O32 1.7100(14) . ? Mo9 O31 1.9167(16) . ? Mo9 O34 1.9168(15) . ? Mo9 O35 2.3230(12) . ? Mo9 O43 2.3852(13) . ? Mo10 O36 1.7037(15) . ? Mo10 O37 1.7082(17) . ? Mo10 O34 1.9155(13) . ? Mo10 O38 1.9265(13) . ? Mo10 O35 2.3401(15) . ? Mo10 O42 2.4072(14) . ? Mo11 O39 1.7005(17) . ? Mo11 O40 1.7026(14) . ? Mo11 O41 1.9194(15) . ? Mo11 O38 1.9225(14) . ? Mo11 O42 2.3333(12) . ? Mo11 O44 2.4033(15) . ? Mo12 O48 1.7019(14) . ? Mo12 O47 1.7134(16) . ? Mo12 O51 1.9088(16) . ? Mo12 O41 1.9247(16) . ? Mo12 O46 2.3108(12) . ? Mo12 O44 2.3906(14) . ? Mn1 O7 1.9438(12) . ? Mn1 O7 1.9438(12) 2_575 ? Mn1 O5 1.9855(14) . ? Mn1 O5 1.9855(14) 2_575 ? Mn1 O3 2.0155(15) 2_575 ? Mn1 O3 2.0155(15) . ? Mn2 O18 1.9489(13) . ? Mn2 O18 1.9489(12) 2_665 ? Mn2 O20 1.9990(14) 2_665 ? Mn2 O20 1.9990(14) . ? Mn2 O22 2.0116(16) 2_665 ? Mn2 O22 2.0116(16) . ? Mn3 O44 1.9044(13) . ? Mn3 O43 1.9085(12) . ? Mn3 O42 1.9550(16) . ? Mn3 O45 1.9660(16) . ? Mn3 O46 2.0921(15) . ? Mn3 O35 2.0999(14) . ? O3 C1 1.443(3) . ? O5 C3 1.440(3) . ? O7 C2 1.440(3) . ? O7 Mo3 2.3948(15) 2_575 ? O8 Mo3 1.9200(15) 2_575 ? O13 C5 1.232(3) . ? O14 C12 1.331(2) . ? O15 C12 1.180(3) . ? O18 C37 1.455(3) . ? O20 C39 1.442(3) 2_665 ? O20 Mo6 2.3866(16) 2_665 ? O21 Mo6 1.9139(14) 2_665 ? O22 C38 1.423(3) . ? O28 C41 1.223(3) . ? O29 C48 1.322(3) . ? O30 C48 1.206(3) . ? O35 C76 1.438(2) . ? O42 C109 1.435(3) . ? O43 C111 1.451(3) . ? O44 C73 1.444(3) . ? O45 C74 1.430(3) . ? O46 C110 1.433(3) . ? O55 C113 1.239(3) . ? O56 C144 1.323(3) . ? O57 C144 1.197(3) . ? O58 C77 1.220(3) . ? O59 C84 1.370(2) . ? O60 C84 1.184(3) . ? O61 C257 1.250(3) . ? O62 C262 1.222(3) . ? O63 C263 1.233(4) . ? O64 C268 1.219(3) . ? O65 C269 1.225(4) . ? O66 C272 1.228(4) . ? O67 C275 1.234(7) . ? O68 C278 1.174(5) . ? O69 C281 1.309(7) . ? O70 C252 1.279(6) . ? O70 C249 1.411(5) . ? O71 C254 1.403(5) . ? O71 C255 1.418(4) . ? O72 C243 1.390(4) . ? O72 C242 1.470(5) . ? O73 C246 1.321(8) . ? O73 C247 1.438(9) . ? O74 C293 1.538(8) . ? O74 C294 1.558(9) . ? O75 C299 1.245(5) . ? O75 C298 1.249(6) . ? O76 C301 1.267(5) . ? N1 C5 1.340(3) . ? N1 C4 1.475(3) . ? N2 C41 1.348(3) . ? N2 C40 1.481(3) . ? N3 C113 1.345(3) . ? N3 C112 1.469(3) . ? N4 C77 1.347(3) . ? N4 C75 1.472(3) . ? N5 C145 1.516(3) . ? N5 C149 1.517(3) . ? N5 C157 1.520(3) . ? N5 C153 1.534(3) . ? N6 C173 1.478(3) . ? N6 C165 1.520(3) . ? N6 C161 1.522(3) . ? N6 C169 1.541(3) . ? N7 C189 1.499(3) . ? N7 C185 1.512(4) . ? N7 C181 1.528(4) . ? N7 C177 1.532(3) . ? N8 C201 1.492(3) . ? N8 C193 1.520(4) . ? N8 C197 1.537(3) . ? N8 C205 1.538(4) . ? N9 C221 1.517(3) . ? N9 C217 1.524(3) . ? N9 C213 1.527(3) . ? N9 C209 1.534(3) . ? N10 C237 1.502(3) . ? N10 C225 1.516(3) . ? N10 C233 1.526(3) . ? N10 C229 1.530(3) . ? N11 C257 1.300(3) . ? N11 C258 1.433(4) . ? N11 C259 1.464(3) . ? N12 C262 1.297(3) . ? N12 C260 1.433(4) . ? N12 C261 1.449(3) . ? N13 C263 1.305(4) . ? N13 C264 1.441(4) . ? N13 C265 1.454(4) . ? N14 C268 1.311(3) . ? N14 C266 1.455(3) . ? N14 C267 1.474(4) . ? N15 C269 1.291(4) . ? N15 C270 1.438(4) . ? N15 C271 1.451(3) . ? N16 C272 1.298(4) . ? N16 C273 1.428(4) . ? N16 C274 1.443(4) . ? N18 C278 1.275(6) . ? N18 C279 1.408(8) . ? N18 C280 1.417(9) . ? C1 C4 1.540(3) . ? C2 C4 1.540(3) . ? C3 C4 1.542(3) 2_575 ? C4 C3 1.542(3) 2_575 ? C5 C6 1.506(3) . ? C6 C11 1.402(3) . ? C6 C7 1.410(3) . ? C7 C8 1.421(3) . ? C7 C13 1.488(3) . ? C8 C9 1.407(3) . ? C8 C19 1.491(3) . ? C9 C10 1.410(3) . ? C9 C25 1.485(3) . ? C10 C11 1.394(3) . ? C10 C36 1.485(3) . ? C11 C12 1.532(3) . ? C13 C14 1.391(4) . ? C13 C18 1.393(4) . ? C14 C15 1.386(4) . ? C15 C16 1.330(4) . ? C16 C17 1.377(4) . ? C17 C18 1.412(4) . ? C19 C24 1.374(4) . ? C19 C20 1.396(3) . ? C20 C21 1.444(4) . ? C21 C22 1.379(4) . ? C22 C23 1.317(3) . ? C23 C24 1.355(4) . ? C25 C30 1.369(3) . ? C25 C26 1.415(3) . ? C26 C27 1.376(4) . ? C27 C28 1.372(3) . ? C28 C29 1.366(4) . ? C29 C30 1.388(4) . ? C31 C36 1.381(3) . ? C31 C32 1.451(4) . ? C32 C33 1.356(4) . ? C33 C34 1.323(4) . ? C34 C35 1.370(4) . ? C35 C36 1.384(3) . ? C37 C40 1.518(3) . ? C38 C40 1.560(3) 2_665 ? C39 O20 1.442(3) 2_665 ? C39 C40 1.534(3) . ? C40 C38 1.560(3) 2_665 ? C41 C42 1.511(3) . ? C42 C43 1.402(3) . ? C42 C47 1.413(3) . ? C43 C44 1.402(3) . ? C43 C49 1.495(3) . ? C44 C45 1.407(3) . ? C44 C60 1.504(3) . ? C45 C46 1.423(3) . ? C45 C61 1.484(4) . ? C46 C47 1.399(3) . ? C46 C67 1.497(3) . ? C47 C48 1.482(3) . ? C49 C50 1.374(4) . ? C49 C54 1.394(4) . ? C50 C51 1.371(4) . ? C51 C52 1.352(5) . ? C52 C53 1.372(5) . ? C53 C54 1.463(4) . ? C55 C60 1.372(4) . ? C55 C56 1.424(4) . ? C56 C57 1.405(3) . ? C57 C58 1.371(4) . ? C58 C59 1.362(4) . ? C59 C60 1.401(3) . ? C61 C62 1.394(3) . ? C61 C66 1.395(3) . ? C62 C63 1.375(4) . ? C63 C64 1.377(4) . ? C64 C65 1.388(4) . ? C65 C66 1.386(4) . ? C67 C72 1.372(3) . ? C67 C68 1.384(3) . ? C68 C69 1.424(4) . ? C69 C70 1.393(3) . ? C70 C71 1.368(4) . ? C71 C72 1.364(4) . ? C73 C75 1.529(3) . ? C74 C75 1.536(3) . ? C75 C76 1.548(3) . ? C77 C83 1.504(3) . ? C78 C79 1.400(3) . ? C78 C83 1.416(3) . ? C78 C85 1.485(3) . ? C79 C80 1.419(3) . ? C79 C91 1.497(3) . ? C80 C81 1.405(3) . ? C80 C97 1.510(3) . ? C81 C82 1.399(3) . ? C81 C103 1.505(3) . ? C82 C83 1.398(3) . ? C82 C84 1.504(3) . ? C85 C86 1.361(4) . ? C85 C90 1.369(4) . ? C86 C87 1.401(4) . ? C87 C88 1.367(4) . ? C88 C89 1.322(4) . ? C89 C90 1.437(4) . ? C91 C92 1.379(4) . ? C91 C96 1.394(3) . ? C92 C93 1.404(3) . ? C93 C94 1.365(3) . ? C94 C95 1.381(4) . ? C95 C96 1.375(3) . ? C97 C98 1.360(3) . ? C97 C102 1.409(3) . ? C98 C99 1.367(4) . ? C99 C100 1.414(3) . ? C100 C101 1.327(4) . ? C101 C102 1.382(4) . ? C103 C104 1.365(3) . ? C103 C108 1.391(3) . ? C104 C105 1.392(4) . ? C105 C106 1.332(4) . ? C106 C107 1.321(4) . ? C107 C108 1.411(4) . ? C109 C112 1.553(3) . ? C110 C112 1.522(3) . ? C111 C112 1.541(3) . ? C113 C114 1.524(3) . ? C114 C119 1.405(3) . ? C114 C115 1.422(3) . ? C115 C116 1.396(3) . ? C115 C144 1.510(3) . ? C116 C117 1.409(3) . ? C116 C143 1.501(3) . ? C117 C118 1.399(3) . ? C117 C132 1.474(3) . ? C118 C119 1.419(3) . ? C118 C126 1.493(3) . ? C119 C120 1.501(3) . ? C120 C125 1.366(3) . ? C120 C121 1.398(3) . ? C121 C122 1.368(4) . ? C122 C123 1.325(4) . ? C123 C124 1.384(4) . ? C124 C125 1.421(4) . ? C126 C131 1.374(3) . ? C126 C127 1.390(4) . ? C127 C128 1.373(3) . ? C128 C129 1.338(3) . ? C129 C130 1.371(4) . ? C130 C131 1.386(3) . ? C132 C137 1.395(3) . ? C132 C133 1.408(3) . ? C133 C134 1.377(4) . ? C134 C135 1.384(3) . ? C135 C136 1.392(4) . ? C136 C137 1.366(4) . ? C138 C143 1.369(3) . ? C138 C139 1.422(4) . ? C139 C140 1.340(4) . ? C140 C141 1.361(4) . ? C141 C142 1.385(4) . ? C142 C143 1.379(4) . ? C145 C146 1.503(3) . ? C146 C147 1.545(4) . ? C147 C148 1.523(4) . ? C149 C150 1.498(4) . ? C150 C151 1.534(4) . ? C151 C152 1.459(6) . ? C153 C154 1.503(4) . ? C154 C155 1.529(4) . ? C155 C156 1.385(8) . ? C157 C158 1.534(4) . ? C158 C159 1.513(4) . ? C159 C160 1.352(6) . ? C161 C162 1.492(4) . ? C162 C163 1.493(4) . ? C163 C164 1.378(7) . ? C165 C166 1.529(4) . ? C166 C167 1.510(4) . ? C167 C168 1.537(4) . ? C169 C170 1.523(4) . ? C170 C171 1.589(4) . ? C171 C172 1.447(7) . ? C173 C174 1.518(4) . ? C174 C175 1.491(4) . ? C175 C176 1.555(5) . ? C177 C178 1.528(4) . ? C178 C179 1.516(4) . ? C179 C180 1.526(6) . ? C181 C182 1.519(5) . ? C182 C183 1.538(6) . ? C183 C184 1.241(7) . ? C185 C186 1.516(5) . ? C186 C187 1.614(5) . ? C187 C188 1.436(6) . ? C189 C190 1.503(4) . ? C190 C191 1.516(4) . ? C191 C192 1.519(4) . ? C193 C194 1.522(4) . ? C194 C195 1.549(4) . ? C195 C196 1.493(4) . ? C197 C198 1.506(3) . ? C198 C199 1.520(4) . ? C199 C200 1.511(4) . ? C201 C202 1.523(4) . ? C202 C203 1.547(4) . ? C203 C204 1.484(5) . ? C205 C206 1.564(5) . ? C206 C207 1.516(6) . ? C207 C208 1.367(6) . ? C209 C210 1.508(3) . ? C210 C211 1.525(4) . ? C211 C212 1.490(3) . ? C213 C214 1.544(3) . ? C214 C215 1.526(4) . ? C215 C216 1.481(4) . ? C217 C218 1.514(4) . ? C218 C219 1.521(3) . ? C219 C220 1.529(4) . ? C221 C222 1.535(3) . ? C222 C223 1.508(3) . ? C223 C224 1.517(4) . ? C225 C226 1.527(3) . ? C226 C227 1.490(3) . ? C227 C228 1.546(4) . ? C229 C230 1.504(4) . ? C230 C231 1.536(4) . ? C231 C232 1.495(4) . ? C233 C234 1.512(3) . ? C234 C235 1.524(3) . ? C235 C236 1.548(4) . ? C237 C238 1.518(3) . ? C238 C239 1.528(4) . ? C239 C240 1.505(4) . ? C241 C242 1.508(7) . ? C243 C244 1.537(6) . ? C245 C246 1.431(8) . ? C247 C248 1.674(11) . ? C249 C250 1.383(6) . ? C251 C252 1.371(7) . ? C253 C254 1.543(6) . ? C255 C256 1.508(5) . ? C275 C276 1.409(9) . ? C294 C295 1.380(10) . ? C297 C298 1.387(7) . ? C299 C300 1.424(6) . ? C301 C302 1.489(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O2 105.76(8) . . ? O1 Mo1 O4 99.50(7) . . ? O2 Mo1 O4 102.49(7) . . ? O1 Mo1 O9 101.71(6) . . ? O2 Mo1 O9 97.53(6) . . ? O4 Mo1 O9 145.51(6) . . ? O1 Mo1 O3 92.59(6) . . ? O2 Mo1 O3 160.24(7) . . ? O4 Mo1 O3 81.14(5) . . ? O9 Mo1 O3 71.07(5) . . ? O1 Mo1 O5 162.43(6) . . ? O2 Mo1 O5 91.03(7) . . ? O4 Mo1 O5 71.21(6) . . ? O9 Mo1 O5 80.71(5) . . ? O3 Mo1 O5 71.56(5) . . ? O6 Mo2 O12 106.40(8) . . ? O6 Mo2 O4 99.46(7) . . ? O12 Mo2 O4 102.09(7) . . ? O6 Mo2 O8 101.07(7) . . ? O12 Mo2 O8 98.80(7) . . ? O4 Mo2 O8 145.09(5) . . ? O6 Mo2 O5 160.79(7) . . ? O12 Mo2 O5 92.18(6) . . ? O4 Mo2 O5 71.28(5) . . ? O8 Mo2 O5 80.32(5) . . ? O6 Mo2 O7 92.16(6) . . ? O12 Mo2 O7 160.55(6) . . ? O4 Mo2 O7 79.98(6) . . ? O8 Mo2 O7 71.34(6) . . ? O5 Mo2 O7 69.97(5) . . ? O11 Mo3 O10 105.20(8) . . ? O11 Mo3 O8 98.67(7) . 2_575 ? O10 Mo3 O8 102.10(7) . 2_575 ? O11 Mo3 O9 102.49(7) . . ? O10 Mo3 O9 98.11(7) . . ? O8 Mo3 O9 145.63(6) 2_575 . ? O11 Mo3 O3 92.90(6) . . ? O10 Mo3 O3 160.72(7) . . ? O8 Mo3 O3 81.25(5) 2_575 . ? O9 Mo3 O3 70.98(5) . . ? O11 Mo3 O7 161.42(6) . 2_575 ? O10 Mo3 O7 92.28(7) . 2_575 ? O8 Mo3 O7 71.00(6) 2_575 2_575 ? O9 Mo3 O7 80.76(6) . 2_575 ? O3 Mo3 O7 70.65(5) . 2_575 ? O26 Mo4 O27 106.01(8) . . ? O26 Mo4 O25 98.88(7) . . ? O27 Mo4 O25 102.54(7) . . ? O26 Mo4 O16 101.30(7) . . ? O27 Mo4 O16 99.13(7) . . ? O25 Mo4 O16 144.88(6) . . ? O26 Mo4 O22 160.52(7) . . ? O27 Mo4 O22 92.53(6) . . ? O25 Mo4 O22 70.67(5) . . ? O16 Mo4 O22 81.14(5) . . ? O26 Mo4 O18 91.80(7) . . ? O27 Mo4 O18 161.04(6) . . ? O25 Mo4 O18 80.54(6) . . ? O16 Mo4 O18 70.42(6) . . ? O22 Mo4 O18 70.63(5) . . ? O17 Mo5 O19 106.36(7) . . ? O17 Mo5 O16 101.37(7) . . ? O19 Mo5 O16 98.49(8) . . ? O17 Mo5 O21 99.18(8) . . ? O19 Mo5 O21 102.65(7) . . ? O16 Mo5 O21 144.87(6) . . ? O17 Mo5 O18 91.86(6) . . ? O19 Mo5 O18 160.70(6) . . ? O16 Mo5 O18 71.10(6) . . ? O21 Mo5 O18 80.09(6) . . ? O17 Mo5 O20 160.70(7) . . ? O19 Mo5 O20 92.26(6) . . ? O16 Mo5 O20 80.35(6) . . ? O21 Mo5 O20 71.15(6) . . ? O18 Mo5 O20 70.33(5) . . ? O24 Mo6 O23 105.62(8) . . ? O24 Mo6 O21 100.34(7) . 2_665 ? O23 Mo6 O21 102.72(7) . 2_665 ? O24 Mo6 O25 101.68(7) . . ? O23 Mo6 O25 97.54(7) . . ? O21 Mo6 O25 144.67(6) 2_665 . ? O24 Mo6 O22 92.89(7) . . ? O23 Mo6 O22 159.97(7) . . ? O21 Mo6 O22 80.89(5) 2_665 . ? O25 Mo6 O22 70.74(5) . . ? O24 Mo6 O20 163.10(7) . 2_665 ? O23 Mo6 O20 90.61(7) . 2_665 ? O21 Mo6 O20 70.84(6) 2_665 2_665 ? O25 Mo6 O20 80.39(6) . 2_665 ? O22 Mo6 O20 71.78(5) . 2_665 ? O49 Mo7 O50 105.13(8) . . ? O49 Mo7 O51 103.95(7) . . ? O50 Mo7 O51 97.92(7) . . ? O49 Mo7 O52 99.03(7) . . ? O50 Mo7 O52 101.22(7) . . ? O51 Mo7 O52 144.94(6) . . ? O49 Mo7 O46 91.61(7) . . ? O50 Mo7 O46 161.72(7) . . ? O51 Mo7 O46 70.41(6) . . ? O52 Mo7 O46 82.94(6) . . ? O49 Mo7 O45 161.61(7) . . ? O50 Mo7 O45 92.00(7) . . ? O51 Mo7 O45 79.74(5) . . ? O52 Mo7 O45 70.55(5) . . ? O46 Mo7 O45 72.45(5) . . ? O54 Mo8 O53 105.67(8) . . ? O54 Mo8 O31 100.06(7) . . ? O53 Mo8 O31 101.09(7) . . ? O54 Mo8 O52 101.83(7) . . ? O53 Mo8 O52 98.28(7) . . ? O31 Mo8 O52 145.49(6) . . ? O54 Mo8 O45 92.70(6) . . ? O53 Mo8 O45 160.84(7) . . ? O31 Mo8 O45 80.57(5) . . ? O52 Mo8 O45 72.09(5) . . ? O54 Mo8 O43 160.41(6) . . ? O53 Mo8 O43 93.35(7) . . ? O31 Mo8 O43 71.09(6) . . ? O52 Mo8 O43 79.54(6) . . ? O45 Mo8 O43 68.93(5) . . ? O33 Mo9 O32 105.50(7) . . ? O33 Mo9 O31 98.79(7) . . ? O32 Mo9 O31 100.98(7) . . ? O33 Mo9 O34 102.92(7) . . ? O32 Mo9 O34 98.33(7) . . ? O31 Mo9 O34 145.77(5) . . ? O33 Mo9 O35 96.08(6) . . ? O32 Mo9 O35 157.80(6) . . ? O31 Mo9 O35 80.43(5) . . ? O34 Mo9 O35 71.28(5) . . ? O33 Mo9 O43 165.73(6) . . ? O32 Mo9 O43 86.80(6) . . ? O31 Mo9 O43 71.26(5) . . ? O34 Mo9 O43 81.96(5) . . ? O35 Mo9 O43 72.56(4) . . ? O36 Mo10 O37 105.19(8) . . ? O36 Mo10 O34 104.39(6) . . ? O37 Mo10 O34 98.10(7) . . ? O36 Mo10 O38 98.79(6) . . ? O37 Mo10 O38 101.21(7) . . ? O34 Mo10 O38 144.61(6) . . ? O36 Mo10 O35 91.62(7) . . ? O37 Mo10 O35 161.98(6) . . ? O34 Mo10 O35 70.91(5) . . ? O38 Mo10 O35 82.19(6) . . ? O36 Mo10 O42 161.30(7) . . ? O37 Mo10 O42 92.02(6) . . ? O34 Mo10 O42 79.82(5) . . ? O38 Mo10 O42 70.17(5) . . ? O35 Mo10 O42 72.32(5) . . ? O39 Mo11 O40 105.64(8) . . ? O39 Mo11 O41 100.10(7) . . ? O40 Mo11 O41 100.43(7) . . ? O39 Mo11 O38 102.06(7) . . ? O40 Mo11 O38 98.90(7) . . ? O41 Mo11 O38 145.30(6) . . ? O39 Mo11 O42 93.17(6) . . ? O40 Mo11 O42 160.59(7) . . ? O41 Mo11 O42 80.51(5) . . ? O38 Mo11 O42 71.94(5) . . ? O39 Mo11 O44 160.81(6) . . ? O40 Mo11 O44 93.02(7) . . ? O41 Mo11 O44 71.54(6) . . ? O38 Mo11 O44 78.93(6) . . ? O42 Mo11 O44 68.71(5) . . ? O48 Mo12 O47 105.11(7) . . ? O48 Mo12 O51 97.91(7) . . ? O47 Mo12 O51 103.16(7) . . ? O48 Mo12 O41 101.26(7) . . ? O47 Mo12 O41 98.55(7) . . ? O51 Mo12 O41 146.05(5) . . ? O48 Mo12 O46 157.56(6) . . ? O47 Mo12 O46 96.65(6) . . ? O51 Mo12 O46 71.38(6) . . ? O41 Mo12 O46 80.50(5) . . ? O48 Mo12 O44 86.70(6) . . ? O47 Mo12 O44 166.24(6) . . ? O51 Mo12 O44 81.73(6) . . ? O41 Mo12 O44 71.76(6) . . ? O46 Mo12 O44 72.50(5) . . ? O7 Mn1 O7 180.000(1) . 2_575 ? O7 Mn1 O5 87.63(5) . . ? O7 Mn1 O5 92.37(5) 2_575 . ? O7 Mn1 O5 92.37(5) . 2_575 ? O7 Mn1 O5 87.63(5) 2_575 2_575 ? O5 Mn1 O5 180.00(7) . 2_575 ? O7 Mn1 O3 87.65(6) . 2_575 ? O7 Mn1 O3 92.35(6) 2_575 2_575 ? O5 Mn1 O3 92.57(6) . 2_575 ? O5 Mn1 O3 87.43(6) 2_575 2_575 ? O7 Mn1 O3 92.35(6) . . ? O7 Mn1 O3 87.65(6) 2_575 . ? O5 Mn1 O3 87.43(6) . . ? O5 Mn1 O3 92.57(6) 2_575 . ? O3 Mn1 O3 180.00(5) 2_575 . ? O18 Mn2 O18 180.00(10) . 2_665 ? O18 Mn2 O20 92.56(6) . 2_665 ? O18 Mn2 O20 87.44(6) 2_665 2_665 ? O18 Mn2 O20 87.44(6) . . ? O18 Mn2 O20 92.56(6) 2_665 . ? O20 Mn2 O20 180.00(12) 2_665 . ? O18 Mn2 O22 92.49(6) . 2_665 ? O18 Mn2 O22 87.51(6) 2_665 2_665 ? O20 Mn2 O22 92.40(6) 2_665 2_665 ? O20 Mn2 O22 87.60(6) . 2_665 ? O18 Mn2 O22 87.51(6) . . ? O18 Mn2 O22 92.49(6) 2_665 . ? O20 Mn2 O22 87.60(6) 2_665 . ? O20 Mn2 O22 92.40(6) . . ? O22 Mn2 O22 180.00(8) 2_665 . ? O44 Mn3 O43 179.50(8) . . ? O44 Mn3 O42 87.69(6) . . ? O43 Mn3 O42 92.72(6) . . ? O44 Mn3 O45 92.21(6) . . ? O43 Mn3 O45 87.39(6) . . ? O42 Mn3 O45 179.88(7) . . ? O44 Mn3 O46 88.04(6) . . ? O43 Mn3 O46 92.23(6) . . ? O42 Mn3 O46 92.60(6) . . ? O45 Mn3 O46 87.45(6) . . ? O44 Mn3 O35 91.78(6) . . ? O43 Mn3 O35 87.95(5) . . ? O42 Mn3 O35 87.34(6) . . ? O45 Mn3 O35 92.61(6) . . ? O46 Mn3 O35 179.81(7) . . ? C1 O3 Mn1 115.89(12) . . ? C1 O3 Mo1 121.39(11) . . ? Mn1 O3 Mo1 100.83(6) . . ? C1 O3 Mo3 121.89(11) . . ? Mn1 O3 Mo3 100.58(6) . . ? Mo1 O3 Mo3 91.40(5) . . ? Mo1 O4 Mo2 122.23(8) . . ? C3 O5 Mn1 116.84(11) . . ? C3 O5 Mo2 121.64(11) . . ? Mn1 O5 Mo2 100.58(6) . . ? C3 O5 Mo1 122.23(12) . . ? Mn1 O5 Mo1 100.17(6) . . ? Mo2 O5 Mo1 89.97(5) . . ? C2 O7 Mn1 117.24(11) . . ? C2 O7 Mo2 120.70(12) . . ? Mn1 O7 Mo2 101.83(6) . . ? C2 O7 Mo3 121.02(13) . 2_575 ? Mn1 O7 Mo3 101.12(6) . 2_575 ? Mo2 O7 Mo3 89.89(5) . 2_575 ? Mo3 O8 Mo2 121.98(8) 2_575 . ? Mo3 O9 Mo1 121.55(7) . . ? Mo5 O16 Mo4 122.41(8) . . ? C37 O18 Mn2 117.51(11) . . ? C37 O18 Mo5 120.27(11) . . ? Mn2 O18 Mo5 101.94(6) . . ? C37 O18 Mo4 120.52(12) . . ? Mn2 O18 Mo4 101.33(6) . . ? Mo5 O18 Mo4 90.35(5) . . ? C39 O20 Mn2 116.14(11) 2_665 . ? C39 O20 Mo5 122.63(11) 2_665 . ? Mn2 O20 Mo5 100.30(6) . . ? C39 O20 Mo6 122.47(12) 2_665 2_665 ? Mn2 O20 Mo6 99.85(6) . 2_665 ? Mo5 O20 Mo6 90.00(5) . 2_665 ? Mo6 O21 Mo5 122.77(8) 2_665 . ? C38 O22 Mn2 115.25(13) . . ? C38 O22 Mo6 122.16(12) . . ? Mn2 O22 Mo6 100.76(6) . . ? C38 O22 Mo4 122.10(11) . . ? Mn2 O22 Mo4 100.53(6) . . ? Mo6 O22 Mo4 91.14(5) . . ? Mo4 O25 Mo6 122.16(8) . . ? Mo9 O31 Mo8 121.91(8) . . ? Mo10 O34 Mo9 122.03(8) . . ? C76 O35 Mn3 114.47(11) . . ? C76 O35 Mo9 122.86(10) . . ? Mn3 O35 Mo9 97.94(5) . . ? C76 O35 Mo10 124.76(12) . . ? Mn3 O35 Mo10 99.13(6) . . ? Mo9 O35 Mo10 91.93(5) . . ? Mo11 O38 Mo10 121.72(8) . . ? Mo11 O41 Mo12 121.52(8) . . ? C109 O42 Mn3 116.72(13) . . ? C109 O42 Mo11 121.30(11) . . ? Mn3 O42 Mo11 102.24(6) . . ? C109 O42 Mo10 120.25(11) . . ? Mn3 O42 Mo10 101.20(6) . . ? Mo11 O42 Mo10 90.32(5) . . ? C111 O43 Mn3 118.30(10) . . ? C111 O43 Mo9 121.44(11) . . ? Mn3 O43 Mo9 101.55(6) . . ? C111 O43 Mo8 119.19(12) . . ? Mn3 O43 Mo8 101.82(6) . . ? Mo9 O43 Mo8 89.24(4) . . ? C73 O44 Mn3 118.74(11) . . ? C73 O44 Mo12 121.54(11) . . ? Mn3 O44 Mo12 101.19(6) . . ? C73 O44 Mo11 119.61(12) . . ? Mn3 O44 Mo11 101.32(6) . . ? Mo12 O44 Mo11 88.81(5) . . ? C74 O45 Mn3 116.19(13) . . ? C74 O45 Mo8 121.04(11) . . ? Mn3 O45 Mo8 101.84(6) . . ? C74 O45 Mo7 121.74(12) . . ? Mn3 O45 Mo7 100.91(6) . . ? Mo8 O45 Mo7 90.26(5) . . ? C110 O46 Mn3 113.63(12) . . ? C110 O46 Mo12 123.41(11) . . ? Mn3 O46 Mo12 98.28(6) . . ? C110 O46 Mo7 124.60(12) . . ? Mn3 O46 Mo7 99.17(6) . . ? Mo12 O46 Mo7 92.16(5) . . ? Mo12 O51 Mo7 122.18(8) . . ? Mo8 O52 Mo7 121.78(8) . . ? C252 O70 C249 137.6(4) . . ? C254 O71 C255 116.2(3) . . ? C243 O72 C242 112.2(3) . . ? C246 O73 C247 110.7(5) . . ? C293 O74 C294 139.4(5) . . ? C299 O75 C298 123.2(4) . . ? C5 N1 C4 128.9(2) . . ? C41 N2 C40 127.8(2) . . ? C113 N3 C112 126.8(2) . . ? C77 N4 C75 126.94(19) . . ? C145 N5 C149 113.2(2) . . ? C145 N5 C157 110.3(2) . . ? C149 N5 C157 108.11(17) . . ? C145 N5 C153 106.16(17) . . ? C149 N5 C153 110.65(19) . . ? C157 N5 C153 108.34(19) . . ? C173 N6 C165 111.4(2) . . ? C173 N6 C161 106.90(18) . . ? C165 N6 C161 111.8(2) . . ? C173 N6 C169 109.6(2) . . ? C165 N6 C169 105.65(17) . . ? C161 N6 C169 111.6(2) . . ? C189 N7 C185 111.8(2) . . ? C189 N7 C181 111.0(2) . . ? C185 N7 C181 106.5(2) . . ? C189 N7 C177 104.46(19) . . ? C185 N7 C177 112.55(19) . . ? C181 N7 C177 110.6(2) . . ? C201 N8 C193 111.8(2) . . ? C201 N8 C197 104.8(2) . . ? C193 N8 C197 112.0(2) . . ? C201 N8 C205 111.7(2) . . ? C193 N8 C205 104.6(2) . . ? C197 N8 C205 112.0(2) . . ? C221 N9 C217 109.44(17) . . ? C221 N9 C213 111.85(16) . . ? C217 N9 C213 107.99(17) . . ? C221 N9 C209 107.31(17) . . ? C217 N9 C209 112.11(16) . . ? C213 N9 C209 108.18(16) . . ? C237 N10 C225 111.35(16) . . ? C237 N10 C233 108.88(18) . . ? C225 N10 C233 109.80(17) . . ? C237 N10 C229 108.60(18) . . ? C225 N10 C229 107.28(18) . . ? C233 N10 C229 110.92(16) . . ? C257 N11 C258 121.6(2) . . ? C257 N11 C259 120.6(2) . . ? C258 N11 C259 117.8(2) . . ? C262 N12 C260 120.8(2) . . ? C262 N12 C261 123.6(2) . . ? C260 N12 C261 115.5(2) . . ? C263 N13 C264 119.2(3) . . ? C263 N13 C265 121.3(3) . . ? C264 N13 C265 119.4(3) . . ? C268 N14 C266 123.5(2) . . ? C268 N14 C267 120.1(2) . . ? C266 N14 C267 116.5(2) . . ? C269 N15 C270 119.2(2) . . ? C269 N15 C271 123.6(2) . . ? C270 N15 C271 117.2(2) . . ? C272 N16 C273 122.1(3) . . ? C272 N16 C274 121.2(3) . . ? C273 N16 C274 116.5(3) . . ? C278 N18 C279 105.0(5) . . ? C278 N18 C280 125.6(4) . . ? C279 N18 C280 126.5(6) . . ? O3 C1 C4 113.09(18) . . ? O7 C2 C4 113.23(15) . . ? O5 C3 C4 112.75(17) . 2_575 ? N1 C4 C2 108.31(15) . . ? N1 C4 C1 102.19(18) . . ? C2 C4 C1 112.11(18) . . ? N1 C4 C3 107.96(17) . 2_575 ? C2 C4 C3 111.6(2) . 2_575 ? C1 C4 C3 114.03(15) . 2_575 ? O13 C5 N1 126.5(2) . . ? O13 C5 C6 119.1(2) . . ? N1 C5 C6 114.3(2) . . ? C11 C6 C7 120.2(2) . . ? C11 C6 C5 119.8(2) . . ? C7 C6 C5 120.0(2) . . ? C6 C7 C8 119.5(2) . . ? C6 C7 C13 119.9(2) . . ? C8 C7 C13 120.6(2) . . ? C9 C8 C7 118.6(2) . . ? C9 C8 C19 119.9(2) . . ? C7 C8 C19 121.6(2) . . ? C8 C9 C10 122.3(2) . . ? C8 C9 C25 119.3(2) . . ? C10 C9 C25 118.44(19) . . ? C11 C10 C9 118.0(2) . . ? C11 C10 C36 120.6(2) . . ? C9 C10 C36 121.4(2) . . ? C10 C11 C6 121.5(2) . . ? C10 C11 C12 119.8(2) . . ? C6 C11 C12 118.7(2) . . ? O15 C12 O14 126.2(2) . . ? O15 C12 C11 122.77(18) . . ? O14 C12 C11 111.0(2) . . ? C14 C13 C18 118.2(2) . . ? C14 C13 C7 119.5(2) . . ? C18 C13 C7 122.3(2) . . ? C15 C14 C13 122.4(3) . . ? C16 C15 C14 120.0(3) . . ? C15 C16 C17 119.4(3) . . ? C16 C17 C18 122.6(3) . . ? C13 C18 C17 117.3(3) . . ? C24 C19 C20 119.1(2) . . ? C24 C19 C8 120.99(19) . . ? C20 C19 C8 119.9(2) . . ? C19 C20 C21 117.0(2) . . ? C22 C21 C20 121.4(2) . . ? C23 C22 C21 117.6(3) . . ? C22 C23 C24 124.2(3) . . ? C23 C24 C19 120.6(2) . . ? C30 C25 C26 116.6(2) . . ? C30 C25 C9 120.5(2) . . ? C26 C25 C9 122.86(19) . . ? C27 C26 C25 121.4(2) . . ? C28 C27 C26 120.6(2) . . ? C29 C28 C27 118.3(3) . . ? C28 C29 C30 121.7(2) . . ? C25 C30 C29 121.1(2) . . ? C36 C31 C32 114.8(2) . . ? C33 C32 C31 122.6(2) . . ? C34 C33 C32 121.0(3) . . ? C33 C34 C35 118.4(3) . . ? C34 C35 C36 123.4(2) . . ? C31 C36 C35 119.6(2) . . ? C31 C36 C10 121.5(2) . . ? C35 C36 C10 118.77(19) . . ? O18 C37 C40 112.39(15) . . ? O22 C38 C40 114.34(19) . 2_665 ? O20 C39 C40 113.16(17) 2_665 . ? N2 C40 C37 109.22(16) . . ? N2 C40 C39 107.29(17) . . ? C37 C40 C39 113.72(19) . . ? N2 C40 C38 101.64(18) . 2_665 ? C37 C40 C38 112.59(17) . 2_665 ? C39 C40 C38 111.52(16) . 2_665 ? O28 C41 N2 124.3(2) . . ? O28 C41 C42 122.5(2) . . ? N2 C41 C42 113.1(2) . . ? C43 C42 C47 121.0(2) . . ? C43 C42 C41 121.8(2) . . ? C47 C42 C41 117.1(2) . . ? C42 C43 C44 118.7(2) . . ? C42 C43 C49 118.7(2) . . ? C44 C43 C49 122.6(2) . . ? C43 C44 C45 121.8(2) . . ? C43 C44 C60 119.2(2) . . ? C45 C44 C60 119.0(2) . . ? C44 C45 C46 118.3(2) . . ? C44 C45 C61 120.1(2) . . ? C46 C45 C61 121.6(2) . . ? C47 C46 C45 120.7(2) . . ? C47 C46 C67 120.9(2) . . ? C45 C46 C67 118.4(2) . . ? C46 C47 C42 119.3(2) . . ? C46 C47 C48 120.8(2) . . ? C42 C47 C48 119.9(2) . . ? O30 C48 O29 124.2(2) . . ? O30 C48 C47 123.1(2) . . ? O29 C48 C47 112.6(2) . . ? C50 C49 C54 119.1(2) . . ? C50 C49 C43 121.4(2) . . ? C54 C49 C43 119.4(2) . . ? C51 C50 C49 124.6(3) . . ? C52 C51 C50 116.1(3) . . ? C51 C52 C53 124.9(3) . . ? C52 C53 C54 117.7(3) . . ? C49 C54 C53 117.6(3) . . ? C60 C55 C56 121.1(2) . . ? C57 C56 C55 118.0(3) . . ? C58 C57 C56 121.0(3) . . ? C59 C58 C57 119.1(2) . . ? C58 C59 C60 123.1(3) . . ? C55 C60 C59 117.6(2) . . ? C55 C60 C44 122.31(19) . . ? C59 C60 C44 120.0(2) . . ? C62 C61 C66 119.2(2) . . ? C62 C61 C45 118.31(19) . . ? C66 C61 C45 122.4(2) . . ? C63 C62 C61 121.1(2) . . ? C62 C63 C64 118.8(3) . . ? C63 C64 C65 121.6(3) . . ? C66 C65 C64 119.2(2) . . ? C65 C66 C61 119.9(3) . . ? C72 C67 C68 117.8(2) . . ? C72 C67 C46 118.6(2) . . ? C68 C67 C46 123.39(19) . . ? C67 C68 C69 118.2(2) . . ? C70 C69 C68 120.0(3) . . ? C71 C70 C69 122.0(3) . . ? C72 C71 C70 115.5(2) . . ? C71 C72 C67 126.5(3) . . ? O44 C73 C75 112.49(15) . . ? O45 C74 C75 114.43(18) . . ? N4 C75 C73 109.15(15) . . ? N4 C75 C74 102.61(18) . . ? C73 C75 C74 111.19(17) . . ? N4 C75 C76 106.69(16) . . ? C73 C75 C76 113.03(18) . . ? C74 C75 C76 113.46(15) . . ? O35 C76 C75 113.09(16) . . ? O58 C77 N4 126.3(2) . . ? O58 C77 C83 119.41(19) . . ? N4 C77 C83 114.32(19) . . ? C79 C78 C83 120.2(2) . . ? C79 C78 C85 120.7(2) . . ? C83 C78 C85 119.1(2) . . ? C78 C79 C80 119.7(2) . . ? C78 C79 C91 120.0(2) . . ? C80 C79 C91 120.3(2) . . ? C81 C80 C79 120.0(2) . . ? C81 C80 C97 119.86(19) . . ? C79 C80 C97 120.11(19) . . ? C82 C81 C80 119.7(2) . . ? C82 C81 C103 121.4(2) . . ? C80 C81 C103 118.9(2) . . ? C83 C82 C81 121.0(2) . . ? C83 C82 C84 119.9(2) . . ? C81 C82 C84 119.1(2) . . ? C82 C83 C78 119.5(2) . . ? C82 C83 C77 120.41(19) . . ? C78 C83 C77 119.93(19) . . ? O60 C84 O59 125.0(2) . . ? O60 C84 C82 125.59(19) . . ? O59 C84 C82 109.38(19) . . ? C86 C85 C90 117.4(2) . . ? C86 C85 C78 120.0(2) . . ? C90 C85 C78 122.6(2) . . ? C85 C86 C87 124.0(3) . . ? C88 C87 C86 117.4(3) . . ? C89 C88 C87 120.7(3) . . ? C88 C89 C90 121.7(3) . . ? C85 C90 C89 118.7(2) . . ? C92 C91 C96 118.1(2) . . ? C92 C91 C79 121.49(18) . . ? C96 C91 C79 120.4(2) . . ? C91 C92 C93 120.4(2) . . ? C94 C93 C92 120.8(3) . . ? C93 C94 C95 118.9(2) . . ? C96 C95 C94 120.9(2) . . ? C95 C96 C91 121.0(2) . . ? C98 C97 C102 118.9(2) . . ? C98 C97 C80 124.02(18) . . ? C102 C97 C80 117.1(2) . . ? C97 C98 C99 120.9(2) . . ? C98 C99 C100 120.3(2) . . ? C101 C100 C99 118.6(2) . . ? C100 C101 C102 122.3(2) . . ? C101 C102 C97 119.1(2) . . ? C104 C103 C108 120.5(2) . . ? C104 C103 C81 119.5(2) . . ? C108 C103 C81 119.95(18) . . ? C103 C104 C105 118.6(2) . . ? C106 C105 C104 122.9(2) . . ? C107 C106 C105 117.3(3) . . ? C106 C107 C108 124.8(3) . . ? C103 C108 C107 115.7(2) . . ? O42 C109 C112 113.49(19) . . ? O46 C110 C112 114.58(18) . . ? O43 C111 C112 112.33(15) . . ? N3 C112 C110 108.31(17) . . ? N3 C112 C111 108.85(15) . . ? C110 C112 C111 112.84(19) . . ? N3 C112 C109 101.66(18) . . ? C110 C112 C109 113.93(16) . . ? C111 C112 C109 110.54(18) . . ? O55 C113 N3 126.0(2) . . ? O55 C113 C114 119.4(2) . . ? N3 C113 C114 114.6(2) . . ? C119 C114 C115 121.0(2) . . ? C119 C114 C113 120.0(2) . . ? C115 C114 C113 118.8(2) . . ? C116 C115 C114 119.5(2) . . ? C116 C115 C144 121.7(2) . . ? C114 C115 C144 118.8(2) . . ? C115 C116 C117 120.2(2) . . ? C115 C116 C143 119.7(2) . . ? C117 C116 C143 120.1(2) . . ? C118 C117 C116 120.1(2) . . ? C118 C117 C132 120.4(2) . . ? C116 C117 C132 119.4(2) . . ? C117 C118 C119 120.86(19) . . ? C117 C118 C126 120.5(2) . . ? C119 C118 C126 118.67(19) . . ? C114 C119 C118 118.3(2) . . ? C114 C119 C120 120.3(2) . . ? C118 C119 C120 121.35(19) . . ? C125 C120 C121 120.9(2) . . ? C125 C120 C119 122.1(2) . . ? C121 C120 C119 117.0(2) . . ? C122 C121 C120 120.7(3) . . ? C123 C122 C121 119.8(3) . . ? C122 C123 C124 121.3(3) . . ? C123 C124 C125 120.6(3) . . ? C120 C125 C124 116.7(3) . . ? C131 C126 C127 118.3(2) . . ? C131 C126 C118 121.8(2) . . ? C127 C126 C118 119.83(19) . . ? C128 C127 C126 119.7(2) . . ? C129 C128 C127 121.6(3) . . ? C128 C129 C130 120.1(3) . . ? C129 C130 C131 119.4(2) . . ? C126 C131 C130 120.9(3) . . ? C137 C132 C133 117.9(2) . . ? C137 C132 C117 121.9(2) . . ? C133 C132 C117 120.28(18) . . ? C134 C133 C132 120.5(2) . . ? C133 C134 C135 120.2(3) . . ? C134 C135 C136 120.2(3) . . ? C137 C136 C135 119.4(2) . . ? C136 C137 C132 121.9(2) . . ? C143 C138 C139 119.0(2) . . ? C140 C139 C138 119.8(2) . . ? C139 C140 C141 123.0(3) . . ? C140 C141 C142 116.5(3) . . ? C143 C142 C141 123.4(2) . . ? C138 C143 C142 118.2(2) . . ? C138 C143 C116 123.2(2) . . ? C142 C143 C116 118.5(2) . . ? O57 C144 O56 123.8(2) . . ? O57 C144 C115 123.0(2) . . ? O56 C144 C115 113.19(19) . . ? C146 C145 N5 115.84(18) . . ? C145 C146 C147 108.52(19) . . ? C148 C147 C146 110.3(2) . . ? C150 C149 N5 114.6(2) . . ? C149 C150 C151 112.2(2) . . ? C152 C151 C150 112.0(3) . . ? C154 C153 N5 115.51(19) . . ? C153 C154 C155 109.4(2) . . ? C156 C155 C154 112.9(3) . . ? N5 C157 C158 116.68(19) . . ? C159 C158 C157 114.4(2) . . ? C160 C159 C158 117.8(4) . . ? C162 C161 N6 114.7(2) . . ? C161 C162 C163 112.6(2) . . ? C164 C163 C162 117.0(4) . . ? N6 C165 C166 115.68(19) . . ? C167 C166 C165 108.8(2) . . ? C166 C167 C168 111.4(2) . . ? C170 C169 N6 115.1(2) . . ? C169 C170 C171 109.6(2) . . ? C172 C171 C170 110.9(3) . . ? N6 C173 C174 115.3(2) . . ? C175 C174 C173 112.3(2) . . ? C174 C175 C176 112.5(3) . . ? C178 C177 N7 114.3(2) . . ? C179 C178 C177 109.2(2) . . ? C178 C179 C180 111.0(3) . . ? C182 C181 N7 117.3(3) . . ? C181 C182 C183 111.9(3) . . ? C184 C183 C182 102.3(5) . . ? N7 C185 C186 115.2(2) . . ? C185 C186 C187 117.4(3) . . ? C188 C187 C186 104.4(3) . . ? N7 C189 C190 117.2(2) . . ? C189 C190 C191 110.0(3) . . ? C190 C191 C192 112.9(3) . . ? N8 C193 C194 114.5(2) . . ? C193 C194 C195 110.2(2) . . ? C196 C195 C194 113.3(2) . . ? C198 C197 N8 116.6(2) . . ? C197 C198 C199 110.3(2) . . ? C200 C199 C198 112.7(3) . . ? N8 C201 C202 117.1(2) . . ? C201 C202 C203 110.7(2) . . ? C204 C203 C202 112.8(3) . . ? N8 C205 C206 116.9(3) . . ? C207 C206 C205 108.3(3) . . ? C208 C207 C206 128.2(4) . . ? C210 C209 N9 115.30(18) . . ? C209 C210 C211 110.8(2) . . ? C212 C211 C210 113.1(2) . . ? N9 C213 C214 114.13(18) . . ? C215 C214 C213 109.9(2) . . ? C216 C215 C214 115.6(2) . . ? C218 C217 N9 115.5(2) . . ? C217 C218 C219 110.9(2) . . ? C218 C219 C220 111.8(2) . . ? N9 C221 C222 115.17(19) . . ? C223 C222 C221 110.4(2) . . ? C222 C223 C224 110.5(2) . . ? N10 C225 C226 114.56(19) . . ? C227 C226 C225 110.5(2) . . ? C226 C227 C228 113.6(2) . . ? C230 C229 N10 116.5(2) . . ? C229 C230 C231 111.0(2) . . ? C232 C231 C230 116.5(2) . . ? C234 C233 N10 114.32(19) . . ? C233 C234 C235 111.7(2) . . ? C234 C235 C236 111.6(2) . . ? N10 C237 C238 116.8(2) . . ? C237 C238 C239 109.8(2) . . ? C240 C239 C238 112.7(2) . . ? O72 C242 C241 105.5(4) . . ? O72 C243 C244 110.0(3) . . ? O73 C246 C245 113.0(6) . . ? O73 C247 C248 100.8(6) . . ? C250 C249 O70 119.6(4) . . ? O70 C252 C251 132.0(5) . . ? O71 C254 C253 110.2(3) . . ? O71 C255 C256 113.7(3) . . ? O61 C257 N11 123.9(3) . . ? O62 C262 N12 124.8(2) . . ? O63 C263 N13 126.9(3) . . ? O64 C268 N14 125.5(3) . . ? O65 C269 N15 127.2(3) . . ? O66 C272 N16 125.6(3) . . ? O67 C275 C276 161.9(5) . . ? O68 C278 N18 130.0(4) . . ? C295 C294 O74 107.4(6) . . ? O75 C298 C297 124.2(5) . . ? O75 C299 C300 118.9(4) . . ? O76 C301 C302 118.5(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.61 _refine_diff_density_min -0.77 _refine_diff_density_rms 0.09