# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Nathan Patmore' _publ_contact_author_email n.patmore@sheffield.ac.uk loop_ _publ_author_name J.Hicks S.Ring N.Patmore data_Mo2NO(py)2.5py _database_code_depnum_ccdc_archive 'CCDC 859556' #TrackingRef '- Mo2EE_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H40 Mo2 N4 O4, 7(C5 H5 N)' _chemical_formula_sum 'C95 H75 Mo2 N11 O4' _chemical_formula_weight 1626.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system Monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' 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 13.501(4) _cell_length_b 20.289(6) _cell_length_c 14.126(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.104(8) _cell_angle_gamma 90.00 _cell_volume 3869(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8896 _cell_measurement_theta_min 26.50 _cell_measurement_theta_max 2.32 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1676 _exptl_absorpt_coefficient_mu 0.387 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9371 _exptl_absorpt_correction_T_max 0.9734 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37994 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.55 _reflns_number_total 8876 _reflns_number_gt 7202 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The following Uiso/Uij restraints were used to model the disordered pyridine solvent molecules: DELU 0.01 0.01 N6 N7 DELU 0.01 0.01 C49 C46 C50 C48 C47 C51 C52 C53 C54 C55 DELU 0.01 0.01 N4 N5 DELU 0.01 0.01 C39 C38 C37 C36 C40 C41 C42 C45 C44 C43 SIMU 0.04 0.08 1.7 N6 N7 SIMU 0.04 0.08 1.7 C49 C46 C50 C48 C47 C51 C52 C53 C54 C55 SIMU 0.04 0.08 1.7 N4 N5 SIMU 0.04 0.08 1.7 C39 C38 C37 C36 C40 C41 C42 C45 C44 C43 EADP N8 C58 EXYZ N8 C58 ; _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^)+(0.0581P)^2^+4.4906P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8876 _refine_ls_number_parameters 591 _refine_ls_number_restraints 220 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1399 _refine_ls_wR_factor_gt 0.1280 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.172 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.50595(2) 0.971646(13) 0.563076(19) 0.02327(9) Uani 1 1 d . . . O1 O 0.52881(17) 1.11738(11) 0.50681(15) 0.0265(5) Uani 1 1 d . . . O2 O 0.34286(17) 1.05046(12) 0.45933(15) 0.0277(5) Uani 1 1 d . . . N1 N 0.54547(19) 1.05789(13) 0.64121(18) 0.0227(5) Uani 1 1 d . . . N2 N 0.3529(2) 0.98950(13) 0.59307(19) 0.0250(6) Uani 1 1 d . . . C1 C 0.5073(3) 1.3354(2) 0.7309(4) 0.0555(12) Uani 1 1 d . . . H1 H 0.4437 1.3215 0.7099 0.067 Uiso 1 1 calc R . . C2 C 0.5182(4) 1.3963(2) 0.7731(4) 0.0611(14) Uani 1 1 d . . . H2 H 0.4624 1.4242 0.7809 0.073 Uiso 1 1 calc R . . C3 C 0.6102(3) 1.4164(2) 0.8039(3) 0.0444(10) Uani 1 1 d . . . H3 H 0.6180 1.4585 0.8321 0.053 Uiso 1 1 calc R . . C4 C 0.6886(3) 1.3767(2) 0.7941(3) 0.0503(11) Uani 1 1 d . . . H4 H 0.7513 1.3904 0.8175 0.060 Uiso 1 1 calc R . . C5 C 0.6796(3) 1.3158(2) 0.7501(3) 0.0495(11) Uani 1 1 d . . . H5 H 0.7364 1.2889 0.7414 0.059 Uiso 1 1 calc R . . C6 C 0.5879(3) 1.29435(17) 0.7188(2) 0.0319(7) Uani 1 1 d . . . C7 C 0.5755(3) 1.23039(18) 0.6772(2) 0.0319(8) Uani 1 1 d . . . C8 C 0.5634(2) 1.17661(17) 0.6439(2) 0.0278(7) Uani 1 1 d . . . C9 C 0.5457(2) 1.11477(16) 0.5960(2) 0.0254(7) Uani 1 1 d . . . C10 C 0.5656(3) 1.05524(17) 0.7408(2) 0.0289(7) Uani 1 1 d . . . C11 C 0.4988(3) 1.0808(2) 0.8059(3) 0.0394(9) Uani 1 1 d . . . H11 H 0.4413 1.1036 0.7849 0.047 Uiso 1 1 calc R . . C12 C 0.5170(4) 1.0728(2) 0.9021(3) 0.0519(11) Uani 1 1 d . . . H12 H 0.4714 1.0900 0.9469 0.062 Uiso 1 1 calc R . . C13 C 0.5999(4) 1.0404(2) 0.9332(3) 0.0531(12) Uani 1 1 d . . . H13 H 0.6117 1.0353 0.9991 0.064 Uiso 1 1 calc R . . C14 C 0.6657(3) 1.0153(2) 0.8687(3) 0.0514(11) Uani 1 1 d . . . H14 H 0.7231 0.9929 0.8905 0.062 Uiso 1 1 calc R . . C15 C 0.6495(3) 1.02225(19) 0.7715(3) 0.0382(8) Uani 1 1 d . . . H15 H 0.6952 1.0046 0.7272 0.046 Uiso 1 1 calc R . . C16 C -0.0533(4) 1.0956(3) 0.5324(4) 0.0715(16) Uani 1 1 d . . . H16 H -0.0368 1.0934 0.4671 0.086 Uiso 1 1 calc R . . C17 C -0.1478(4) 1.1143(3) 0.5580(5) 0.086(2) Uani 1 1 d . . . H17 H -0.1955 1.1249 0.5109 0.103 Uiso 1 1 calc R . . C18 C -0.1723(3) 1.1175(2) 0.6525(4) 0.0585(13) Uani 1 1 d . . . H18 H -0.2368 1.1308 0.6713 0.070 Uiso 1 1 calc R . . C19 C -0.1035(3) 1.1014(2) 0.7179(4) 0.0537(11) Uani 1 1 d . . . H19 H -0.1203 1.1027 0.7832 0.064 Uiso 1 1 calc R . . C20 C -0.0092(3) 1.0829(2) 0.6916(3) 0.0499(10) Uani 1 1 d . . . H20 H 0.0383 1.0719 0.7387 0.060 Uiso 1 1 calc R . . C21 C 0.0166(3) 1.0802(2) 0.5979(3) 0.0420(9) Uani 1 1 d . . . C22 C 0.1161(3) 1.0611(2) 0.5704(3) 0.0410(9) Uani 1 1 d . . . C23 C 0.1997(3) 1.04480(19) 0.5531(3) 0.0354(8) Uani 1 1 d . . . C24 C 0.3020(3) 1.02746(17) 0.5342(2) 0.0297(7) Uani 1 1 d . . . C25 C 0.3045(3) 0.9666(2) 0.6769(3) 0.0389(9) Uani 1 1 d . . . C26 C 0.2926(3) 0.8986(2) 0.6888(3) 0.0502(11) Uani 1 1 d . . . H26 H 0.3113 0.8694 0.6393 0.060 Uiso 1 1 calc R . . C27 C 0.2539(4) 0.8736(3) 0.7715(4) 0.0694(16) Uani 1 1 d . . . H27 H 0.2474 0.8273 0.7796 0.083 Uiso 1 1 calc R . . C28 C 0.2245(4) 0.9164(4) 0.8434(4) 0.0768(19) Uani 1 1 d . . . H28 H 0.1972 0.8993 0.9002 0.092 Uiso 1 1 calc R . . C29 C 0.2353(3) 0.9845(3) 0.8318(3) 0.0632(14) Uani 1 1 d . . . H29 H 0.2152 1.0138 0.8806 0.076 Uiso 1 1 calc R . . C30 C 0.2753(3) 1.0090(2) 0.7487(3) 0.0458(10) Uani 1 1 d . . . H30 H 0.2828 1.0552 0.7408 0.055 Uiso 1 1 calc R . . N8 N 0.5632(7) 0.4602(6) 0.5430(8) 0.148(4) Uani 0.50 1 d P A 1 C56 C 0.5721(7) 0.5265(6) 0.5539(8) 0.136(4) Uani 1 1 d . . . H56 H 0.6242 0.5451 0.5903 0.164 Uiso 1 1 calc R A 1 C57 C 0.4933(7) 0.4371(5) 0.4873(10) 0.143(4) Uani 1 1 d . . . H57 H 0.4908 0.3909 0.4768 0.171 Uiso 1 1 calc R A 1 C58 C 0.5632(7) 0.4602(6) 0.5430(8) 0.148(4) Uani 0.50 1 d P A 2 H58 H 0.6069 0.4311 0.5751 0.177 Uiso 0.50 1 calc PR A 2 N4 N 0.3519(5) 0.2150(4) 0.8541(6) 0.074(4) Uani 0.477(13) 1 d PG B 1 C40 C 0.2787(8) 0.1833(5) 0.8016(6) 0.064(4) Uani 0.477(13) 1 d PGU B 1 H40 H 0.2946 0.1639 0.7424 0.076 Uiso 0.477(13) 1 calc PR B 1 C39 C 0.1824(7) 0.1802(7) 0.8360(9) 0.103(5) Uani 0.477(13) 1 d PGU B 1 H39 H 0.1324 0.1586 0.8001 0.124 Uiso 0.477(13) 1 calc PR B 1 C38 C 0.1593(6) 0.2086(7) 0.9227(9) 0.111(6) Uani 0.477(13) 1 d PGU B 1 H38 H 0.0934 0.2064 0.9461 0.133 Uiso 0.477(13) 1 calc PR B 1 C37 C 0.2324(8) 0.2402(7) 0.9751(6) 0.105(6) Uani 0.477(13) 1 d PGU B 1 H37 H 0.2166 0.2596 1.0343 0.126 Uiso 0.477(13) 1 calc PR B 1 C36 C 0.3287(7) 0.2434(6) 0.9408(6) 0.102(6) Uani 0.477(13) 1 d PGU B 1 H36 H 0.3787 0.2650 0.9766 0.123 Uiso 0.477(13) 1 calc PR B 1 N5 N 0.1800(9) 0.1970(9) 0.9683(5) 0.218(14) Uani 0.523(13) 1 d PG B 2 C41 C 0.2816(9) 0.2043(10) 0.9806(7) 0.139(7) Uani 0.523(13) 1 d PGU B 2 H41 H 0.3085 0.2083 1.0425 0.167 Uiso 0.523(13) 1 calc PR B 2 C42 C 0.3438(6) 0.2057(9) 0.9023(10) 0.151(7) Uani 0.523(13) 1 d PGU B 2 H42 H 0.4132 0.2107 0.9107 0.182 Uiso 0.523(13) 1 calc PR B 2 C43 C 0.3043(8) 0.1999(9) 0.8117(8) 0.114(6) Uani 0.523(13) 1 d PGU B 2 H43 H 0.3468 0.2009 0.7582 0.137 Uiso 0.523(13) 1 calc PR B 2 C44 C 0.2028(9) 0.1927(8) 0.7994(5) 0.107(5) Uani 0.523(13) 1 d PGU B 2 H44 H 0.1758 0.1887 0.7375 0.128 Uiso 0.523(13) 1 calc PR B 2 C45 C 0.1406(6) 0.1912(8) 0.8777(7) 0.122(6) Uani 0.523(13) 1 d PGU B 2 H45 H 0.0712 0.1863 0.8693 0.146 Uiso 0.523(13) 1 calc PR B 2 N6 N 0.1684(8) 0.8099(4) 0.0574(7) 0.063(3) Uani 0.76(2) 1 d P C 1 N7 N 0.334(2) 0.7342(19) 0.018(2) 0.065(8) Uani 0.24(2) 1 d P C 2 C46 C 0.2638(12) 0.8099(5) 0.0790(7) 0.059(3) Uani 0.76(2) 1 d PU C 1 H46 H 0.2857 0.8399 0.1262 0.070 Uiso 0.76(2) 1 calc PR C 1 C47 C 0.3327(9) 0.7700(8) 0.0386(10) 0.076(3) Uani 0.76(2) 1 d PU C 1 H47 H 0.4005 0.7713 0.0566 0.092 Uiso 0.76(2) 1 calc PR C 1 C48 C 0.2963(11) 0.7254(6) -0.0336(12) 0.076(4) Uani 0.76(2) 1 d PU C 1 H48 H 0.3400 0.6954 -0.0639 0.091 Uiso 0.76(2) 1 calc PR C 1 C49 C 0.1985(12) 0.7270(6) -0.0573(9) 0.066(3) Uani 0.76(2) 1 d PU C 1 H49 H 0.1728 0.6995 -0.1059 0.079 Uiso 0.76(2) 1 calc PR C 1 C50 C 0.1395(9) 0.7688(7) -0.0096(8) 0.064(3) Uani 0.76(2) 1 d PU C 1 H50 H 0.0711 0.7687 -0.0255 0.076 Uiso 0.76(2) 1 calc PR C 1 C51 C 0.307(3) 0.7923(19) 0.071(3) 0.058(8) Uani 0.24(2) 1 d PU C 2 H51 H 0.3506 0.8094 0.1176 0.070 Uiso 0.24(2) 1 calc PR C 2 C52 C 0.219(3) 0.8227(16) 0.055(3) 0.056(7) Uani 0.24(2) 1 d PU C 2 H52 H 0.2040 0.8623 0.0881 0.067 Uiso 0.24(2) 1 calc PR C 2 C53 C 0.155(3) 0.7994(19) -0.003(3) 0.064(7) Uani 0.24(2) 1 d PU C 2 H53 H 0.0937 0.8213 -0.0114 0.076 Uiso 0.24(2) 1 calc PR C 2 C54 C 0.173(3) 0.749(2) -0.047(3) 0.055(6) Uani 0.24(2) 1 d PU C 2 H54 H 0.1219 0.7341 -0.0880 0.066 Uiso 0.24(2) 1 calc PR C 2 C55 C 0.255(4) 0.714(2) -0.045(3) 0.065(8) Uani 0.24(2) 1 d PU C 2 H55 H 0.2618 0.6769 -0.0850 0.078 Uiso 0.24(2) 1 calc PR C 2 N3 N 0.5293(2) 0.88577(16) 0.7064(2) 0.0375(7) Uani 1 1 d . . . C31 C 0.4987(3) 0.8908(2) 0.7957(3) 0.0454(10) Uani 1 1 d . . . H31 H 0.4786 0.9329 0.8180 0.054 Uiso 1 1 calc R . . C32 C 0.4947(4) 0.8384(2) 0.8573(3) 0.0579(13) Uani 1 1 d . . . H32 H 0.4722 0.8445 0.9204 0.069 Uiso 1 1 calc R . . C33 C 0.5234(4) 0.7777(2) 0.8267(3) 0.0571(12) Uani 1 1 d . . . H33 H 0.5208 0.7407 0.8678 0.069 Uiso 1 1 calc R . . C34 C 0.5563(3) 0.7710(2) 0.7352(3) 0.0519(11) Uani 1 1 d . . . H34 H 0.5770 0.7295 0.7115 0.062 Uiso 1 1 calc R . . C35 C 0.5582(3) 0.8266(2) 0.6788(3) 0.0445(10) Uani 1 1 d . . . H35 H 0.5819 0.8220 0.6159 0.053 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 0.03142(15) 0.01813(14) 0.02026(14) -0.00013(11) -0.00065(10) 0.00158(11) O1 0.0360(12) 0.0194(11) 0.0243(11) -0.0014(9) 0.0005(9) 0.0012(9) O2 0.0314(12) 0.0269(12) 0.0247(11) 0.0009(10) 0.0011(9) 0.0050(9) N1 0.0249(13) 0.0219(13) 0.0213(13) -0.0026(11) 0.0015(10) 0.0008(10) N2 0.0316(14) 0.0217(14) 0.0218(13) -0.0014(10) 0.0040(11) -0.0042(11) C1 0.039(2) 0.046(3) 0.082(3) -0.030(2) -0.012(2) 0.0029(18) C2 0.056(3) 0.045(3) 0.082(4) -0.032(2) -0.009(2) 0.011(2) C3 0.055(2) 0.030(2) 0.048(2) -0.0122(18) 0.0003(19) -0.0080(18) C4 0.048(2) 0.035(2) 0.067(3) -0.009(2) -0.017(2) -0.0075(18) C5 0.044(2) 0.034(2) 0.070(3) -0.013(2) -0.012(2) 0.0000(17) C6 0.0370(19) 0.0277(18) 0.0310(18) -0.0027(14) 0.0007(14) -0.0049(14) C7 0.0320(18) 0.0324(19) 0.0313(18) 0.0005(15) -0.0013(14) -0.0002(14) C8 0.0289(16) 0.0264(17) 0.0281(17) -0.0041(14) 0.0002(13) 0.0025(13) C9 0.0250(15) 0.0231(16) 0.0282(17) -0.0047(13) -0.0009(13) -0.0007(12) C10 0.0336(17) 0.0270(17) 0.0260(16) -0.0013(14) -0.0019(13) -0.0061(14) C11 0.046(2) 0.038(2) 0.034(2) -0.0029(17) 0.0016(16) -0.0004(17) C12 0.071(3) 0.052(3) 0.033(2) -0.0067(19) 0.011(2) -0.005(2) C13 0.079(3) 0.053(3) 0.028(2) 0.0023(18) -0.011(2) -0.014(2) C14 0.054(3) 0.050(3) 0.049(3) 0.009(2) -0.022(2) -0.005(2) C15 0.039(2) 0.037(2) 0.038(2) 0.0009(17) -0.0051(16) -0.0015(16) C16 0.056(3) 0.108(5) 0.050(3) -0.022(3) -0.006(2) 0.030(3) C17 0.058(3) 0.111(5) 0.088(4) -0.034(4) -0.034(3) 0.030(3) C18 0.033(2) 0.048(3) 0.095(4) -0.012(3) 0.006(2) 0.0015(19) C19 0.051(3) 0.044(3) 0.066(3) 0.007(2) 0.018(2) 0.004(2) C20 0.041(2) 0.044(2) 0.064(3) 0.004(2) 0.005(2) 0.0039(18) C21 0.035(2) 0.038(2) 0.053(2) -0.0063(19) -0.0034(17) -0.0018(16) C22 0.043(2) 0.037(2) 0.043(2) -0.0033(17) -0.0014(17) 0.0056(17) C23 0.0352(19) 0.037(2) 0.0335(19) -0.0014(15) 0.0011(15) 0.0022(15) C24 0.0338(17) 0.0258(17) 0.0296(17) -0.0031(14) -0.0011(13) -0.0011(14) C25 0.0311(18) 0.046(2) 0.040(2) 0.0061(18) -0.0032(15) -0.0043(16) C26 0.045(2) 0.046(3) 0.060(3) 0.018(2) -0.011(2) -0.0113(19) C27 0.052(3) 0.077(4) 0.079(4) 0.042(3) -0.010(3) -0.019(3) C28 0.051(3) 0.116(5) 0.063(3) 0.049(4) 0.002(2) -0.025(3) C29 0.048(3) 0.102(5) 0.040(2) 0.006(3) 0.009(2) -0.002(3) C30 0.043(2) 0.056(3) 0.038(2) 0.0012(19) 0.0041(17) -0.0007(19) N8 0.110(7) 0.177(11) 0.157(8) 0.041(7) -0.005(6) -0.045(7) C56 0.089(6) 0.136(9) 0.183(10) -0.069(8) -0.016(6) -0.017(6) C57 0.072(5) 0.101(7) 0.255(13) -0.032(8) 0.023(7) -0.019(5) C58 0.110(7) 0.177(11) 0.157(8) 0.041(7) -0.005(6) -0.045(7) N4 0.115(10) 0.048(6) 0.059(7) -0.006(5) -0.012(6) 0.015(6) C40 0.037(6) 0.105(10) 0.049(6) -0.038(6) -0.013(4) 0.006(6) C39 0.072(8) 0.149(13) 0.089(11) -0.013(10) 0.019(8) -0.008(9) C38 0.087(9) 0.170(16) 0.076(12) -0.005(10) 0.027(8) 0.027(9) C37 0.097(10) 0.146(15) 0.073(8) -0.025(8) 0.025(7) 0.046(9) C36 0.087(8) 0.153(16) 0.067(9) -0.030(9) 0.009(7) 0.044(9) N5 0.140(15) 0.36(4) 0.156(17) -0.18(2) -0.017(12) -0.047(17) C41 0.101(12) 0.24(2) 0.078(8) -0.032(12) -0.002(8) -0.029(12) C42 0.096(10) 0.26(2) 0.099(11) -0.031(15) 0.008(7) 0.005(13) C43 0.067(8) 0.197(16) 0.078(8) -0.049(11) 0.007(7) -0.008(10) C44 0.075(8) 0.174(13) 0.071(8) 0.017(9) 0.029(6) -0.012(9) C45 0.103(9) 0.218(16) 0.044(8) -0.010(9) 0.027(7) 0.023(11) N6 0.074(6) 0.058(4) 0.056(5) 0.007(3) 0.009(5) 0.007(4) N7 0.070(15) 0.062(18) 0.064(17) 0.011(15) -0.003(12) 0.000(14) C46 0.081(9) 0.044(6) 0.051(4) 0.006(4) 0.011(5) -0.003(5) C47 0.064(6) 0.068(8) 0.097(8) -0.003(6) 0.014(5) -0.003(6) C48 0.078(7) 0.061(6) 0.088(9) -0.011(5) 0.021(7) 0.008(6) C49 0.078(8) 0.055(7) 0.063(5) -0.003(5) 0.015(5) -0.011(6) C50 0.063(5) 0.078(8) 0.050(5) 0.007(6) 0.007(4) 0.000(5) C51 0.058(16) 0.054(17) 0.063(15) -0.001(12) -0.002(13) 0.022(12) C52 0.056(17) 0.044(12) 0.068(15) 0.013(10) -0.006(13) 0.010(11) C53 0.057(12) 0.058(14) 0.076(17) 0.005(15) -0.001(11) -0.009(11) C54 0.052(13) 0.054(15) 0.060(15) 0.015(11) 0.005(12) -0.014(12) C55 0.073(19) 0.065(15) 0.058(13) 0.005(12) -0.008(16) 0.003(15) N3 0.0412(17) 0.0342(17) 0.0370(17) 0.0052(14) -0.0012(14) 0.0001(14) C31 0.064(3) 0.032(2) 0.040(2) 0.0021(17) -0.0069(19) -0.0047(18) C32 0.091(4) 0.049(3) 0.034(2) 0.005(2) -0.002(2) -0.012(2) C33 0.083(3) 0.042(3) 0.046(3) 0.018(2) -0.003(2) -0.002(2) C34 0.063(3) 0.036(2) 0.056(3) 0.008(2) 0.007(2) 0.010(2) C35 0.050(2) 0.037(2) 0.046(2) 0.0124(18) 0.0025(18) 0.0043(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 2.111(2) 3_676 ? Mo1 O2 2.114(2) 3_676 ? Mo1 Mo1 2.1269(7) 3_676 ? Mo1 N1 2.136(3) . ? Mo1 N2 2.141(3) . ? O1 C9 1.282(4) . ? O1 Mo1 2.111(2) 3_676 ? O2 C24 1.282(4) . ? O2 Mo1 2.114(2) 3_676 ? N1 C9 1.319(4) . ? N1 C10 1.433(4) . ? N2 C24 1.325(4) . ? N2 C25 1.431(5) . ? C1 C2 1.380(6) . ? C1 C6 1.381(5) . ? C1 H1 0.9500 . ? C2 C3 1.378(6) . ? C2 H2 0.9500 . ? C3 C4 1.337(6) . ? C3 H3 0.9500 . ? C4 C5 1.388(6) . ? C4 H4 0.9500 . ? C5 C6 1.384(5) . ? C5 H5 0.9500 . ? C6 C7 1.434(5) . ? C7 C8 1.200(5) . ? C8 C9 1.445(4) . ? C10 C15 1.385(5) . ? C10 C11 1.390(5) . ? C11 C12 1.391(6) . ? C11 H11 0.9500 . ? C12 C13 1.369(7) . ? C12 H12 0.9500 . ? C13 C14 1.371(7) . ? C13 H13 0.9500 . ? C14 C15 1.398(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.357(6) . ? C16 C17 1.380(7) . ? C16 H16 0.9500 . ? C17 C18 1.377(8) . ? C17 H17 0.9500 . ? C18 C19 1.350(7) . ? C18 H18 0.9500 . ? C19 C20 1.379(6) . ? C19 H19 0.9500 . ? C20 C21 1.369(6) . ? C20 H20 0.9500 . ? C21 C22 1.452(5) . ? C22 C23 1.202(5) . ? C23 C24 1.450(5) . ? C25 C30 1.388(6) . ? C25 C26 1.398(6) . ? C26 C27 1.378(7) . ? C26 H26 0.9500 . ? C27 C28 1.394(9) . ? C27 H27 0.9500 . ? C28 C29 1.399(8) . ? C28 H28 0.9500 . ? C29 C30 1.386(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? N8 C57 1.314(13) . ? N8 C56 1.358(12) . ? C56 C57 1.289(14) 3_666 ? C56 H56 0.9500 . ? C57 C56 1.289(14) 3_666 ? C57 H57 0.9500 . ? N4 C40 1.3900 . ? N4 C36 1.3900 . ? C40 C39 1.3900 . ? C40 H40 0.9500 . ? C39 C38 1.3900 . ? C39 H39 0.9500 . ? C38 C37 1.3900 . ? C38 H38 0.9500 . ? C37 C36 1.3900 . ? C37 H37 0.9500 . ? C36 H36 0.9500 . ? N5 C41 1.3900 . ? N5 C45 1.3900 . ? C41 C42 1.3900 . ? C41 H41 0.9500 . ? C42 C43 1.3900 . ? C42 H42 0.9500 . ? C43 C44 1.3900 . ? C43 H43 0.9500 . ? C44 C45 1.3900 . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? N6 C50 1.319(13) . ? N6 C46 1.323(13) . ? N7 C55 1.45(4) . ? N7 C51 1.45(4) . ? C46 C47 1.359(14) . ? C46 H46 0.9500 . ? C47 C48 1.449(16) . ? C47 H47 0.9500 . ? C48 C49 1.362(16) . ? C48 H48 0.9500 . ? C49 C50 1.346(14) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.35(4) . ? C51 H51 0.9500 . ? C52 C53 1.27(5) . ? C52 H52 0.9500 . ? C53 C54 1.22(5) . ? C53 H53 0.9500 . ? C54 C55 1.31(5) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? N3 C35 1.321(5) . ? N3 C31 1.331(5) . ? C31 C32 1.375(6) . ? C31 H31 0.9500 . ? C32 C33 1.362(7) . ? C32 H32 0.9500 . ? C33 C34 1.373(6) . ? C33 H33 0.9500 . ? C34 C35 1.381(6) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O2 87.84(9) 3_676 3_676 ? O1 Mo1 Mo1 93.13(6) 3_676 3_676 ? O2 Mo1 Mo1 93.49(6) 3_676 3_676 ? O1 Mo1 N1 176.16(9) 3_676 . ? O2 Mo1 N1 90.62(9) 3_676 . ? Mo1 Mo1 N1 90.47(7) 3_676 . ? O1 Mo1 N2 91.35(9) 3_676 . ? O2 Mo1 N2 176.30(9) 3_676 . ? Mo1 Mo1 N2 90.16(7) 3_676 . ? N1 Mo1 N2 89.97(10) . . ? C9 O1 Mo1 117.6(2) . 3_676 ? C24 O2 Mo1 117.6(2) . 3_676 ? C9 N1 C10 120.5(3) . . ? C9 N1 Mo1 117.9(2) . . ? C10 N1 Mo1 121.5(2) . . ? C24 N2 C25 118.1(3) . . ? C24 N2 Mo1 118.3(2) . . ? C25 N2 Mo1 123.4(2) . . ? C2 C1 C6 120.6(4) . . ? C2 C1 H1 119.7 . . ? C6 C1 H1 119.7 . . ? C3 C2 C1 119.8(4) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C4 C3 C2 120.2(4) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.9(4) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 120.0(4) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C1 C6 C5 118.4(4) . . ? C1 C6 C7 120.3(3) . . ? C5 C6 C7 121.3(3) . . ? C8 C7 C6 178.5(4) . . ? C7 C8 C9 174.8(4) . . ? O1 C9 N1 120.8(3) . . ? O1 C9 C8 116.9(3) . . ? N1 C9 C8 122.3(3) . . ? C15 C10 C11 120.3(3) . . ? C15 C10 N1 118.6(3) . . ? C11 C10 N1 120.9(3) . . ? C10 C11 C12 119.3(4) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 120.9(4) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 119.6(4) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C15 121.0(4) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C10 C15 C14 118.9(4) . . ? C10 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C21 C16 C17 121.7(5) . . ? C21 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C18 C17 C16 119.4(5) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C19 C18 C17 119.1(4) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 121.0(5) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C21 C20 C19 120.5(4) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C16 C21 C20 118.2(4) . . ? C16 C21 C22 121.4(4) . . ? C20 C21 C22 120.4(4) . . ? C23 C22 C21 176.2(4) . . ? C22 C23 C24 177.7(4) . . ? O2 C24 N2 120.4(3) . . ? O2 C24 C23 118.3(3) . . ? N2 C24 C23 121.3(3) . . ? C30 C25 C26 119.4(4) . . ? C30 C25 N2 122.2(4) . . ? C26 C25 N2 118.2(4) . . ? C27 C26 C25 120.6(5) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 119.8(5) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C29 120.0(5) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 119.6(5) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C25 120.5(5) . . ? C29 C30 H30 119.7 . . ? C25 C30 H30 119.7 . . ? C57 N8 C56 119.0(10) . . ? C57 C56 N8 117.2(9) 3_666 . ? C57 C56 H56 121.4 3_666 . ? N8 C56 H56 121.4 . . ? C56 C57 N8 123.7(10) 3_666 . ? C56 C57 H57 118.1 3_666 . ? N8 C57 H57 118.1 . . ? C40 N4 C36 120.0 . . ? N4 C40 C39 120.0 . . ? N4 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C38 C39 C40 120.0 . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C38 C37 120.0 . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C36 C37 C38 120.0 . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C37 C36 N4 120.0 . . ? C37 C36 H36 120.0 . . ? N4 C36 H36 120.0 . . ? C41 N5 C45 120.0 . . ? N5 C41 C42 120.0 . . ? N5 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C43 C42 C41 120.0 . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 120.0 . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C43 C44 C45 120.0 . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 N5 120.0 . . ? C44 C45 H45 120.0 . . ? N5 C45 H45 120.0 . . ? C50 N6 C46 116.8(8) . . ? C55 N7 C51 111(3) . . ? N6 C46 C47 124.8(10) . . ? N6 C46 H46 117.6 . . ? C47 C46 H46 117.6 . . ? C46 C47 C48 115.8(10) . . ? C46 C47 H47 122.1 . . ? C48 C47 H47 122.1 . . ? C49 C48 C47 119.0(10) . . ? C49 C48 H48 120.5 . . ? C47 C48 H48 120.5 . . ? C50 C49 C48 117.8(11) . . ? C50 C49 H49 121.1 . . ? C48 C49 H49 121.1 . . ? N6 C50 C49 125.6(10) . . ? N6 C50 H50 117.2 . . ? C49 C50 H50 117.2 . . ? C52 C51 N7 121(3) . . ? C52 C51 H51 119.7 . . ? N7 C51 H51 119.7 . . ? C53 C52 C51 122(3) . . ? C53 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? C54 C53 C52 121(4) . . ? C54 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? C53 C54 C55 127(4) . . ? C53 C54 H54 116.3 . . ? C55 C54 H54 116.3 . . ? C54 C55 N7 119(4) . . ? C54 C55 H55 120.6 . . ? N7 C55 H55 120.6 . . ? C35 N3 C31 116.2(3) . . ? N3 C31 C32 123.6(4) . . ? N3 C31 H31 118.2 . . ? C32 C31 H31 118.2 . . ? C33 C32 C31 119.1(4) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C32 C33 C34 118.7(4) . . ? C32 C33 H33 120.6 . . ? C34 C33 H33 120.6 . . ? C33 C34 C35 117.9(4) . . ? C33 C34 H34 121.0 . . ? C35 C34 H34 121.0 . . ? N3 C35 C34 124.5(4) . . ? N3 C35 H35 117.8 . . ? C34 C35 H35 117.8 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.468 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.133 #===END data_Mo2NS.4(toluene) _database_code_depnum_ccdc_archive 'CCDC 859557' #TrackingRef '- Mo2EE_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H40 Mo2 N4 S4, 4(C7 H8)' _chemical_formula_sum 'C88 H72 Mo2 N4 S4' _chemical_formula_weight 1505.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 26.8014(14) _cell_length_b 26.8014(14) _cell_length_c 10.1004(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7255.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4076 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 27.50 _exptl_crystal_description Rod _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 0.511 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9319 _exptl_absorpt_correction_T_max 0.9603 _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 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44580 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8266 _reflns_number_gt 6074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.in this case the absolute structure parameter is not meaningful. The structure showed intermediate values the flack parameter. We believe that a merohedral twin or a partial mix of enantiomers is present, the configuration refined gives the lowest value for the flack parameter. To this end we omitted the flack value. The following Uiso restraints were used to model the disorder in the ligand (C1-C3) and toluene solvent molecules: DELU C3 C2 C1 SIMU 0.02 C31 C32 C33 C34 C35 C36 SIMU 0.02 C31A C32A C33A C34A C35A C36A SIMU 0.02 C38 C39 C40 C41 C42 C43 SIMU 0.02 C38A C39A C40A C41A C42A C43A SIMU 0.02 C39A C44A C43A C44A ; _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^)+(0.0595P)^2^+36.3205P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 8266 _refine_ls_number_parameters 383 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1479 _refine_ls_wR_factor_gt 0.1276 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3942(3) 0.4632(3) 0.9713(9) 0.0203(19) Uani 1 1 d U . . C2 C 0.3440(3) 0.4452(3) 0.9553(8) 0.0212(18) Uani 1 1 d U . . C3 C 0.3029(3) 0.4298(3) 0.9565(8) 0.0247(18) Uani 1 1 d U . . C4 C 0.2532(3) 0.4087(3) 0.9557(8) 0.0238(18) Uani 1 1 d . . . C5 C 0.2319(2) 0.3931(3) 1.0762(7) 0.0333(15) Uani 1 1 d . . . H5 H 0.2497 0.3965 1.1569 0.040 Uiso 1 1 calc R . . C6 C 0.1844(2) 0.3728(3) 1.0745(8) 0.0371(16) Uani 1 1 d . . . H6 H 0.1695 0.3620 1.1548 0.045 Uiso 1 1 calc R . . C7 C 0.1586(3) 0.3681(3) 0.9566(10) 0.038(2) Uani 1 1 d . . . H7 H 0.1260 0.3541 0.9570 0.046 Uiso 1 1 calc R . . C8 C 0.1793(3) 0.3833(3) 0.8397(8) 0.0403(17) Uani 1 1 d . . . H8 H 0.1613 0.3794 0.7592 0.048 Uiso 1 1 calc R . . C9 C 0.2266(3) 0.4043(3) 0.8386(8) 0.0370(16) Uani 1 1 d . . . H9 H 0.2408 0.4157 0.7578 0.044 Uiso 1 1 calc R . . C10 C 0.4104(2) 0.4584(3) 0.7387(10) 0.0244(16) Uani 1 1 d . . . C11 C 0.4099(2) 0.4932(2) 0.6390(7) 0.0287(14) Uani 1 1 d . . . H11 H 0.4179 0.5269 0.6578 0.034 Uiso 1 1 calc R . . C12 C 0.3976(3) 0.4792(3) 0.5107(7) 0.0344(15) Uani 1 1 d . . . H12 H 0.3971 0.5033 0.4416 0.041 Uiso 1 1 calc R . . C13 C 0.3862(2) 0.4300(3) 0.4849(7) 0.0352(16) Uani 1 1 d . . . H13 H 0.3769 0.4202 0.3979 0.042 Uiso 1 1 calc R . . C14 C 0.3880(2) 0.3949(2) 0.5845(7) 0.0312(14) Uani 1 1 d . . . H14 H 0.3812 0.3609 0.5648 0.037 Uiso 1 1 calc R . . C15 C 0.3999(2) 0.4087(2) 0.7141(6) 0.0283(14) Uani 1 1 d . . . H15 H 0.4008 0.3846 0.7833 0.034 Uiso 1 1 calc R . . C16 C 0.6054(3) 0.0360(3) 0.2807(7) 0.0193(19) Uani 1 1 d . . . C17 C 0.6541(3) 0.0564(3) 0.2980(8) 0.0240(19) Uani 1 1 d . . . C18 C 0.6952(3) 0.0749(3) 0.3045(9) 0.0238(18) Uani 1 1 d . . . C19 C 0.7447(3) 0.0946(3) 0.3108(9) 0.0285(19) Uani 1 1 d . . . C20 C 0.7535(3) 0.1447(3) 0.2845(9) 0.052(3) Uani 1 1 d . . . H20 H 0.7266 0.1660 0.2611 0.062 Uiso 1 1 calc R . . C21 C 0.8019(3) 0.1639(3) 0.2926(10) 0.058(3) Uani 1 1 d . . . H21 H 0.8074 0.1982 0.2742 0.070 Uiso 1 1 calc R . . C22 C 0.8412(3) 0.1346(3) 0.3260(9) 0.034(2) Uani 1 1 d . . . H22 H 0.8739 0.1480 0.3315 0.041 Uiso 1 1 calc R . . C23 C 0.8325(2) 0.0842(3) 0.3522(9) 0.046(2) Uani 1 1 d . . . H23 H 0.8596 0.0631 0.3753 0.055 Uiso 1 1 calc R . . C24 C 0.7848(2) 0.0648(3) 0.3449(9) 0.044(2) Uani 1 1 d . . . H24 H 0.7795 0.0305 0.3636 0.053 Uiso 1 1 calc R . . C25 C 0.5952(2) 0.0261(3) 0.5150(8) 0.0223(15) Uani 1 1 d . . . C26 C 0.6389(2) 0.0017(2) 0.5465(6) 0.0248(13) Uani 1 1 d . . . H26 H 0.6565 -0.0165 0.4807 0.030 Uiso 1 1 calc R . . C27 C 0.6569(2) 0.0040(2) 0.6761(6) 0.0266(13) Uani 1 1 d . . . H27 H 0.6869 -0.0130 0.6984 0.032 Uiso 1 1 calc R . . C28 C 0.6313(3) 0.0309(3) 0.7733(6) 0.0278(14) Uani 1 1 d . . . H28 H 0.6442 0.0335 0.8606 0.033 Uiso 1 1 calc R . . C29 C 0.5862(3) 0.0540(3) 0.7393(7) 0.0347(16) Uani 1 1 d . . . H29 H 0.5678 0.0716 0.8046 0.042 Uiso 1 1 calc R . . C30 C 0.5687(2) 0.0512(3) 0.6122(7) 0.0325(15) Uani 1 1 d . . . H30 H 0.5379 0.0667 0.5903 0.039 Uiso 1 1 calc R . . C31 C 0.4736(4) 0.2666(5) 0.5691(9) 0.057(5) Uiso 0.515(15) 1 d PGU A 1 C32 C 0.4253(5) 0.2477(5) 0.5663(10) 0.070(6) Uiso 0.515(15) 1 d PGU A 1 H32 H 0.4127 0.2330 0.4876 0.083 Uiso 0.515(15) 1 calc PR A 1 C33 C 0.3955(4) 0.2503(5) 0.6788(12) 0.063(5) Uiso 0.515(15) 1 d PGU A 1 H33 H 0.3625 0.2374 0.6769 0.075 Uiso 0.515(15) 1 calc PR A 1 C34 C 0.4140(4) 0.2718(5) 0.7940(10) 0.056(5) Uiso 0.515(15) 1 d PGU A 1 H34 H 0.3937 0.2736 0.8709 0.067 Uiso 0.515(15) 1 calc PR A 1 C35 C 0.4623(4) 0.2907(4) 0.7968(9) 0.039(4) Uiso 0.515(15) 1 d PGU A 1 H35 H 0.4750 0.3054 0.8755 0.046 Uiso 0.515(15) 1 calc PR A 1 C36 C 0.4921(3) 0.2881(4) 0.6843(11) 0.055(5) Uiso 0.515(15) 1 d PGU A 1 H36 H 0.5251 0.3010 0.6862 0.065 Uiso 0.515(15) 1 calc PR A 1 C37 C 0.5037(12) 0.2662(12) 0.442(3) 0.118(11) Uiso 0.515(15) 1 d P A 1 H37A H 0.5368 0.2803 0.4588 0.177 Uiso 0.515(15) 1 calc PR A 1 H37B H 0.4865 0.2863 0.3749 0.177 Uiso 0.515(15) 1 calc PR A 1 H37C H 0.5071 0.2318 0.4102 0.177 Uiso 0.515(15) 1 calc PR A 1 C31A C 0.3574(9) 0.2715(9) 0.698(3) 0.134(11) Uiso 0.485(15) 1 d PGU A 2 C32A C 0.3789(11) 0.2600(9) 0.576(2) 0.140(11) Uiso 0.485(15) 1 d PGU A 2 H32A H 0.3584 0.2508 0.5035 0.168 Uiso 0.485(15) 1 calc PR A 2 C33A C 0.4304(12) 0.2621(10) 0.561(2) 0.162(13) Uiso 0.485(15) 1 d PGU A 2 H33A H 0.4452 0.2542 0.4783 0.194 Uiso 0.485(15) 1 calc PR A 2 C34A C 0.4604(8) 0.2756(10) 0.668(3) 0.144(11) Uiso 0.485(15) 1 d PGU A 2 H34A H 0.4956 0.2770 0.6574 0.172 Uiso 0.485(15) 1 calc PR A 2 C35A C 0.4388(10) 0.2871(9) 0.789(2) 0.123(10) Uiso 0.485(15) 1 d PGU A 2 H35A H 0.4593 0.2964 0.8618 0.148 Uiso 0.485(15) 1 calc PR A 2 C36A C 0.3873(11) 0.2851(9) 0.804(2) 0.126(10) Uiso 0.485(15) 1 d PGU A 2 H36A H 0.3726 0.2929 0.8870 0.151 Uiso 0.485(15) 1 calc PR A 2 C37A C 0.304(2) 0.273(2) 0.719(6) 0.25(3) Uiso 0.485(15) 1 d P A 2 H37D H 0.2972 0.2822 0.8114 0.370 Uiso 0.485(15) 1 calc PR A 2 H37E H 0.2894 0.2408 0.6993 0.370 Uiso 0.485(15) 1 calc PR A 2 H37F H 0.2893 0.2987 0.6606 0.370 Uiso 0.485(15) 1 calc PR A 2 C38 C 0.6965(8) 0.2317(8) 0.515(2) 0.176(11) Uiso 0.670(15) 1 d PGU B 3 C39 C 0.6922(8) 0.1820(8) 0.553(2) 0.139(9) Uiso 0.670(15) 1 d PGU B 3 H39 H 0.7213 0.1627 0.5690 0.167 Uiso 0.670(15) 1 calc PR B 3 C40 C 0.6453(9) 0.1605(6) 0.568(2) 0.160(10) Uiso 0.670(15) 1 d PGU B 3 H40 H 0.6424 0.1266 0.5934 0.192 Uiso 0.670(15) 1 calc PR B 3 C41 C 0.6027(7) 0.1888(9) 0.544(2) 0.162(10) Uiso 0.670(15) 1 d PGU B 3 H41 H 0.5707 0.1741 0.5541 0.194 Uiso 0.670(15) 1 calc PR B 3 C42 C 0.6070(8) 0.2384(8) 0.506(2) 0.199(12) Uiso 0.670(15) 1 d PGU B 3 H42 H 0.5779 0.2577 0.4905 0.239 Uiso 0.670(15) 1 calc PR B 3 C43 C 0.6539(10) 0.2599(6) 0.492(2) 0.176(11) Uiso 0.670(15) 1 d PGU B 3 H43 H 0.6568 0.2939 0.4661 0.211 Uiso 0.670(15) 1 calc PR B 3 C44 C 0.7427(8) 0.2568(9) 0.508(2) 0.118(8) Uiso 0.670(15) 1 d P B 3 H44A H 0.7370 0.2918 0.4849 0.177 Uiso 0.670(15) 1 calc PR B 3 H44B H 0.7637 0.2411 0.4410 0.177 Uiso 0.670(15) 1 calc PR B 3 H44C H 0.7593 0.2550 0.5947 0.177 Uiso 0.670(15) 1 calc PR B 3 C38A C 0.5595(6) 0.2194(8) 0.512(2) 0.074(9) Uiso 0.330(15) 1 d PGU B 4 C39A C 0.5914(8) 0.2591(6) 0.538(2) 0.069(8) Uiso 0.330(15) 1 d PGU B 4 H39A H 0.5786 0.2921 0.5437 0.083 Uiso 0.330(15) 1 calc PR B 4 C40A C 0.6421(7) 0.2506(6) 0.556(2) 0.094(10) Uiso 0.330(15) 1 d PGU B 4 H40A H 0.6639 0.2777 0.5745 0.113 Uiso 0.330(15) 1 calc PR B 4 C41A C 0.6609(6) 0.2023(7) 0.548(2) 0.049(7) Uiso 0.330(15) 1 d PGU B 4 H41A H 0.6955 0.1965 0.5609 0.059 Uiso 0.330(15) 1 calc PR B 4 C42A C 0.6290(8) 0.1626(6) 0.522(2) 0.071(8) Uiso 0.330(15) 1 d PGU B 4 H42A H 0.6419 0.1297 0.5166 0.086 Uiso 0.330(15) 1 calc PR B 4 C43A C 0.5783(7) 0.1712(7) 0.504(3) 0.084(9) Uiso 0.330(15) 1 d PGU B 4 H43A H 0.5565 0.1441 0.4858 0.101 Uiso 0.330(15) 1 calc PR B 4 C44A C 0.5160(15) 0.2402(16) 0.498(5) 0.097(12) Uiso 0.330(15) 1 d P B 4 H44D H 0.4910 0.2145 0.4789 0.145 Uiso 0.330(15) 1 calc PR B 4 H44E H 0.5171 0.2642 0.4248 0.145 Uiso 0.330(15) 1 calc PR B 4 H44F H 0.5070 0.2576 0.5800 0.145 Uiso 0.330(15) 1 calc PR B 4 N1 N 0.4252(2) 0.4727(2) 0.8720(8) 0.0206(16) Uani 1 1 d . . . N2 N 0.5756(2) 0.0241(2) 0.3821(6) 0.0188(15) Uani 1 1 d . . . S1 S 0.41279(7) 0.47325(7) 1.1327(2) 0.0212(5) Uani 1 1 d . . . S2 S 0.58602(7) 0.03032(7) 0.1204(2) 0.0203(5) Uani 1 1 d . . . Mo1 Mo 0.5000 0.5000 0.89591(9) 0.0176(2) Uani 1 2 d S . . Mo2 Mo 0.5000 0.0000 0.35480(8) 0.0158(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.014(3) 0.010(4) 0.037(5) 0.001(3) 0.004(3) 0.009(3) C2 0.018(4) 0.017(4) 0.028(5) 0.002(3) -0.004(3) 0.000(3) C3 0.022(4) 0.025(4) 0.027(4) 0.004(3) -0.001(3) 0.004(3) C4 0.016(4) 0.021(4) 0.034(4) 0.002(3) -0.001(3) -0.001(3) C5 0.020(3) 0.041(4) 0.040(4) 0.007(3) -0.001(3) -0.004(3) C6 0.021(3) 0.044(4) 0.046(4) 0.012(3) 0.007(3) -0.005(3) C7 0.015(4) 0.029(4) 0.071(7) 0.008(4) -0.005(4) -0.006(3) C8 0.029(4) 0.045(4) 0.047(5) -0.003(4) -0.010(3) -0.013(3) C9 0.029(4) 0.041(4) 0.041(4) 0.000(3) -0.004(3) -0.008(3) C10 0.009(3) 0.028(4) 0.036(4) 0.001(3) -0.005(3) 0.004(2) C11 0.027(3) 0.022(3) 0.038(4) 0.001(3) -0.002(3) -0.003(3) C12 0.034(4) 0.037(4) 0.033(4) 0.008(3) 0.000(3) -0.001(3) C13 0.022(3) 0.053(5) 0.030(4) -0.014(3) -0.001(3) 0.003(3) C14 0.030(3) 0.029(3) 0.034(4) -0.010(3) 0.003(3) -0.004(3) C15 0.020(3) 0.030(4) 0.035(4) -0.001(3) 0.002(2) -0.002(3) C16 0.020(4) 0.022(4) 0.016(5) -0.002(3) -0.002(3) -0.008(3) C17 0.016(4) 0.027(4) 0.029(5) 0.003(3) 0.007(3) 0.002(3) C18 0.019(4) 0.019(4) 0.034(4) 0.001(3) 0.000(3) 0.000(3) C19 0.019(4) 0.025(4) 0.041(5) 0.006(3) 0.006(3) -0.002(3) C20 0.029(4) 0.029(4) 0.097(8) 0.021(4) -0.025(4) -0.008(3) C21 0.035(4) 0.040(5) 0.099(8) 0.022(4) -0.022(4) -0.022(4) C22 0.021(4) 0.043(5) 0.038(5) -0.011(4) -0.001(3) -0.009(3) C23 0.014(3) 0.038(4) 0.085(6) 0.003(4) -0.003(3) 0.005(3) C24 0.019(3) 0.027(4) 0.088(6) 0.012(4) -0.006(4) -0.003(3) C25 0.016(3) 0.030(4) 0.021(3) -0.002(3) -0.001(3) -0.002(3) C26 0.020(3) 0.025(3) 0.029(3) 0.000(2) 0.004(2) 0.000(2) C27 0.024(3) 0.032(4) 0.024(3) 0.002(2) -0.003(2) -0.001(3) C28 0.027(4) 0.038(4) 0.018(3) 0.000(2) 0.000(2) -0.008(3) C29 0.029(4) 0.050(5) 0.024(3) -0.014(3) 0.003(3) 0.007(3) C30 0.023(3) 0.042(4) 0.033(4) -0.003(3) 0.003(3) 0.008(3) N1 0.014(3) 0.010(3) 0.038(4) 0.005(3) 0.003(3) 0.008(2) N2 0.020(3) 0.025(3) 0.011(3) -0.004(3) 0.000(3) -0.001(3) S1 0.0150(9) 0.0168(9) 0.0319(13) 0.0043(8) 0.0000(8) -0.0003(7) S2 0.0206(10) 0.0228(10) 0.0174(11) -0.0024(8) 0.0023(8) -0.0028(7) Mo1 0.0118(5) 0.0121(5) 0.0289(6) 0.000 0.000 -0.0003(4) Mo2 0.0153(5) 0.0186(5) 0.0136(4) 0.000 0.000 0.0003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.326(10) . ? C1 C2 1.440(10) . ? C1 S1 1.726(9) . ? C2 C3 1.177(10) . ? C3 C4 1.446(10) . ? C4 C9 1.385(10) . ? C4 C5 1.408(10) . ? C5 C6 1.383(9) . ? C5 H5 0.9500 . ? C6 C7 1.383(11) . ? C6 H6 0.9500 . ? C7 C8 1.367(11) . ? C7 H7 0.9500 . ? C8 C9 1.389(9) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.372(10) . ? C10 C15 1.386(10) . ? C10 N1 1.454(12) . ? C11 C12 1.388(10) . ? C11 H11 0.9500 . ? C12 C13 1.380(10) . ? C12 H12 0.9500 . ? C13 C14 1.379(10) . ? C13 H13 0.9500 . ? C14 C15 1.397(9) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 N2 1.337(9) . ? C16 C17 1.425(11) . ? C16 S2 1.707(7) . ? C17 C18 1.210(10) . ? C18 C19 1.430(11) . ? C19 C24 1.382(10) . ? C19 C20 1.389(11) . ? C20 C21 1.397(10) . ? C20 H20 0.9500 . ? C21 C22 1.358(12) . ? C21 H21 0.9500 . ? C22 C23 1.395(11) . ? C22 H22 0.9500 . ? C23 C24 1.382(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.379(9) . ? C25 C30 1.386(10) . ? C25 N2 1.442(10) . ? C26 C27 1.396(8) . ? C26 H26 0.9500 . ? C27 C28 1.399(9) . ? C27 H27 0.9500 . ? C28 C29 1.399(10) . ? C28 H28 0.9500 . ? C29 C30 1.369(10) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C31 C37 1.52(3) . ? C32 C33 1.3900 . ? C32 H32 0.9500 . ? C33 C34 1.3900 . ? C33 H33 0.9500 . ? C34 C35 1.3900 . ? C34 H34 0.9500 . ? C35 C36 1.3900 . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C31A C32A 1.3900 . ? C31A C36A 1.3900 . ? C31A C37A 1.45(6) . ? C32A C33A 1.3900 . ? C32A H32A 0.9500 . ? C33A C34A 1.3900 . ? C33A H33A 0.9500 . ? C34A C35A 1.3900 . ? C34A H34A 0.9500 . ? C35A C36A 1.3900 . ? C35A H35A 0.9500 . ? C36A H36A 0.9500 . ? C37A H37D 0.9800 . ? C37A H37E 0.9800 . ? C37A H37F 0.9800 . ? C38 C39 1.3900 . ? C38 C43 1.3900 . ? C38 C44 1.41(3) . ? C39 C40 1.3900 . ? C39 H39 0.9500 . ? C40 C41 1.3900 . ? C40 H40 0.9500 . ? C41 C42 1.3900 . ? C41 H41 0.9500 . ? C42 C43 1.3900 . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C38A C44A 1.30(4) . ? C38A C39A 1.3900 . ? C38A C43A 1.3900 . ? C39A C40A 1.3900 . ? C39A H39A 0.9500 . ? C40A C41A 1.3900 . ? C40A H40A 0.9500 . ? C41A C42A 1.3900 . ? C41A H41A 0.9500 . ? C42A C43A 1.3900 . ? C42A H42A 0.9500 . ? C43A H43A 0.9500 . ? C44A H44D 0.9800 . ? C44A H44E 0.9800 . ? C44A H44F 0.9800 . ? N1 Mo1 2.149(6) . ? N2 Mo2 2.144(6) . ? S1 Mo1 2.4618(19) 3_567 ? S2 Mo2 2.4572(19) 7 ? Mo1 Mo1 2.1026(18) 3_567 ? Mo1 N1 2.149(6) 2_665 ? Mo1 S1 2.4618(19) 4_657 ? Mo1 S1 2.4618(19) 3_567 ? Mo2 Mo2 2.1171(16) 7 ? Mo2 N2 2.144(6) 2_655 ? Mo2 S2 2.4572(19) 8_545 ? Mo2 S2 2.4572(19) 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 N1 C1 C2 124.4(8) . . ? N1 C1 S1 120.3(6) . . ? C2 C1 S1 115.3(6) . . ? C3 C2 C1 172.9(9) . . ? C2 C3 C4 177.4(9) . . ? C9 C4 C5 120.3(7) . . ? C9 C4 C3 120.7(7) . . ? C5 C4 C3 118.9(7) . . ? C6 C5 C4 118.6(7) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C5 C6 C7 120.5(7) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 120.8(7) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 119.9(7) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C4 C9 C8 119.8(7) . . ? C4 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C15 121.3(8) . . ? C11 C10 N1 120.3(6) . . ? C15 C10 N1 118.3(7) . . ? C10 C11 C12 120.4(6) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 119.1(7) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C12 120.5(7) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.8(6) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C10 C15 C14 118.0(7) . . ? C10 C15 H15 121.0 . . ? C14 C15 H15 121.0 . . ? N2 C16 C17 123.0(7) . . ? N2 C16 S2 121.5(5) . . ? C17 C16 S2 115.4(6) . . ? C18 C17 C16 175.8(9) . . ? C17 C18 C19 177.4(9) . . ? C24 C19 C20 118.3(7) . . ? C24 C19 C18 121.3(7) . . ? C20 C19 C18 120.4(7) . . ? C19 C20 C21 120.2(7) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 121.4(8) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 118.5(7) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? C24 C23 C22 120.6(7) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C19 C24 C23 120.9(7) . . ? C19 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C26 C25 C30 120.1(7) . . ? C26 C25 N2 120.4(7) . . ? C30 C25 N2 119.5(6) . . ? C25 C26 C27 119.3(6) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C26 C27 C28 120.7(6) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C29 C28 C27 118.6(6) . . ? C29 C28 H28 120.7 . . ? C27 C28 H28 120.7 . . ? C30 C29 C28 120.2(6) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C25 121.0(6) . . ? C29 C30 H30 119.5 . . ? C25 C30 H30 119.5 . . ? C32 C31 C36 120.0 . . ? C32 C31 C37 118.4(14) . . ? C36 C31 C37 121.4(14) . . ? C31 C32 C33 120.0 . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C31 C37 H37A 109.5 . . ? C31 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C31 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C32A C31A C36A 120.0 . . ? C32A C31A C37A 123(3) . . ? C36A C31A C37A 117(3) . . ? C31A C32A C33A 120.0 . . ? C31A C32A H32A 120.0 . . ? C33A C32A H32A 120.0 . . ? C34A C33A C32A 120.0 . . ? C34A C33A H33A 120.0 . . ? C32A C33A H33A 120.0 . . ? C35A C34A C33A 120.0 . . ? C35A C34A H34A 120.0 . . ? C33A C34A H34A 120.0 . . ? C36A C35A C34A 120.0 . . ? C36A C35A H35A 120.0 . . ? C34A C35A H35A 120.0 . . ? C35A C36A C31A 120.0 . . ? C35A C36A H36A 120.0 . . ? C31A C36A H36A 120.0 . . ? C31A C37A H37D 109.5 . . ? C31A C37A H37E 109.5 . . ? H37D C37A H37E 109.5 . . ? C31A C37A H37F 109.5 . . ? H37D C37A H37F 109.5 . . ? H37E C37A H37F 109.5 . . ? C39 C38 C43 120.0 . . ? C39 C38 C44 123(2) . . ? C43 C38 C44 117(2) . . ? C40 C39 C38 120.0 . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C41 120.0 . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C42 C41 C40 120.0 . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C42 C43 C38 120.0 . . ? C42 C43 H43 120.0 . . ? C38 C43 H43 120.0 . . ? C38 C44 H44A 109.5 . . ? C38 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C38 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C44A C38A C39A 104(2) . . ? C44A C38A C43A 136(2) . . ? C39A C38A C43A 120.0 . . ? C38A C39A C40A 120.0 . . ? C38A C39A H39A 120.0 . . ? C40A C39A H39A 120.0 . . ? C39A C40A C41A 120.0 . . ? C39A C40A H40A 120.0 . . ? C41A C40A H40A 120.0 . . ? C42A C41A C40A 120.0 . . ? C42A C41A H41A 120.0 . . ? C40A C41A H41A 120.0 . . ? C43A C42A C41A 120.0 . . ? C43A C42A H42A 120.0 . . ? C41A C42A H42A 120.0 . . ? C42A C43A C38A 120.0 . . ? C42A C43A H43A 120.0 . . ? C38A C43A H43A 120.0 . . ? C38A C44A H44D 109.5 . . ? C38A C44A H44E 109.5 . . ? H44D C44A H44E 109.5 . . ? C38A C44A H44F 109.5 . . ? H44D C44A H44F 109.5 . . ? H44E C44A H44F 109.5 . . ? C1 N1 C10 118.7(6) . . ? C1 N1 Mo1 124.3(6) . . ? C10 N1 Mo1 116.6(5) . . ? C16 N2 C25 119.1(6) . . ? C16 N2 Mo2 122.6(5) . . ? C25 N2 Mo2 118.3(5) . . ? C1 S1 Mo1 102.0(3) . 3_567 ? C16 S2 Mo2 102.6(3) . 7 ? Mo1 Mo1 N1 96.5(2) 3_567 . ? Mo1 Mo1 N1 96.5(2) 3_567 2_665 ? N1 Mo1 N1 167.1(4) . 2_665 ? Mo1 Mo1 S1 96.75(6) 3_567 4_657 ? N1 Mo1 S1 86.30(16) . 4_657 ? N1 Mo1 S1 92.18(15) 2_665 4_657 ? Mo1 Mo1 S1 96.75(6) 3_567 3_567 ? N1 Mo1 S1 92.18(15) . 3_567 ? N1 Mo1 S1 86.30(16) 2_665 3_567 ? S1 Mo1 S1 166.50(11) 4_657 3_567 ? Mo2 Mo2 N2 97.38(17) 7 2_655 ? Mo2 Mo2 N2 97.38(17) 7 . ? N2 Mo2 N2 165.2(3) 2_655 . ? Mo2 Mo2 S2 95.84(5) 7 8_545 ? N2 Mo2 S2 87.51(17) 2_655 8_545 ? N2 Mo2 S2 90.99(17) . 8_545 ? Mo2 Mo2 S2 95.84(5) 7 7 ? N2 Mo2 S2 90.99(17) 2_655 7 ? N2 Mo2 S2 87.51(17) . 7 ? S2 Mo2 S2 168.32(11) 8_545 7 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.405 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.116 #===END data_Mo2OO(THF)2 _database_code_depnum_ccdc_archive 'CCDC 859558' #TrackingRef '- Mo2EE_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H20 Mo2 O8, 2(C4 H8 O)' _chemical_formula_sum 'C44 H36 Mo2 O10' _chemical_formula_weight 916.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.8160(6) _cell_length_b 12.8292(4) _cell_length_c 17.2278(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.032(2) _cell_angle_gamma 90.00 _cell_volume 4158.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9886 _cell_measurement_theta_min 2.165 _cell_measurement_theta_max 27.462 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8740 _exptl_absorpt_correction_T_max 0.9431 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53498 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9550 _reflns_number_gt 8426 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The following Uij restraints were used to model the disordered THF molecules: SADI O10 C41 O10 C44 O10 C41A O10 C44A SADI C41 C44 C41A C44A SADI C41 C42 C41A C42A C43 C44 C43A C44A SADI C42 C43 C42A C43A ; _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^+29.9170P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9550 _refine_ls_number_parameters 499 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1434 _refine_ls_wR_factor_gt 0.1406 _refine_ls_goodness_of_fit_ref 1.271 _refine_ls_restrained_S_all 1.275 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.28092(2) 0.54851(4) 0.30739(2) 0.02129(11) Uani 1 1 d . . . Mo2 Mo 0.22149(2) 0.50953(4) 0.20759(2) 0.02136(11) Uani 1 1 d . . . O1 O 0.24106(19) 0.7020(3) 0.3052(2) 0.0253(8) Uani 1 1 d . . . O2 O 0.17809(19) 0.6601(3) 0.2000(2) 0.0265(8) Uani 1 1 d . . . O3 O 0.1983(2) 0.5007(3) 0.3811(2) 0.0313(9) Uani 1 1 d . . . O4 O 0.13466(19) 0.4604(3) 0.2740(2) 0.0279(8) Uani 1 1 d . . . O5 O 0.32427(19) 0.3980(3) 0.3148(2) 0.0283(8) Uani 1 1 d . . . O6 O 0.26162(19) 0.3554(3) 0.2090(2) 0.0267(8) Uani 1 1 d . . . O7 O 0.36810(19) 0.5968(3) 0.2410(2) 0.0272(8) Uani 1 1 d . . . O8 O 0.3053(2) 0.5565(3) 0.1338(2) 0.0310(9) Uani 1 1 d . . . O9 O 0.3430(3) 0.6125(6) 0.4294(3) 0.075(2) Uani 1 1 d . . . O10 O 0.1681(3) 0.4561(5) 0.0769(3) 0.0621(16) Uani 1 1 d D . . C1 C 0.1980(3) 0.7249(5) 0.2513(3) 0.0270(11) Uani 1 1 d . . . C2 C 0.1695(3) 0.8297(5) 0.2483(3) 0.0302(12) Uani 1 1 d . . . C3 C 0.1426(3) 0.9140(5) 0.2468(3) 0.0314(12) Uani 1 1 d . . . C4 C 0.1105(3) 1.0157(4) 0.2483(3) 0.0292(12) Uani 1 1 d . . . C5 C 0.1500(3) 1.1045(5) 0.2303(4) 0.0416(15) Uani 1 1 d . . . H5 H 0.1980 1.0982 0.2140 0.050 Uiso 1 1 calc R . . C6 C 0.1189(4) 1.2016(5) 0.2365(5) 0.0458(17) Uani 1 1 d . . . H6 H 0.1458 1.2622 0.2245 0.055 Uiso 1 1 calc R . . C7 C 0.0493(3) 1.2115(5) 0.2597(4) 0.0391(14) Uani 1 1 d . . . H7 H 0.0287 1.2787 0.2652 0.047 Uiso 1 1 calc R . . C8 C 0.0100(3) 1.1244(5) 0.2748(4) 0.0395(14) Uani 1 1 d . . . H8 H -0.0385 1.1314 0.2894 0.047 Uiso 1 1 calc R . . C9 C 0.0397(3) 1.0262(5) 0.2693(4) 0.0342(13) Uani 1 1 d . . . H9 H 0.0118 0.9661 0.2797 0.041 Uiso 1 1 calc R . . C10 C 0.1421(3) 0.4646(4) 0.3473(3) 0.0260(11) Uani 1 1 d . . . C11 C 0.0853(3) 0.4245(5) 0.3959(4) 0.0363(13) Uani 1 1 d . . . C12 C 0.0387(3) 0.3835(5) 0.4326(4) 0.0366(14) Uani 1 1 d . . . C13 C -0.0164(3) 0.3330(5) 0.4751(3) 0.0321(12) Uani 1 1 d . . . C14 C -0.0729(3) 0.2858(6) 0.4348(4) 0.0386(14) Uani 1 1 d . . . H14 H -0.0757 0.2910 0.3799 0.046 Uiso 1 1 calc R . . C15 C -0.1240(3) 0.2319(6) 0.4753(4) 0.0416(15) Uani 1 1 d . . . H15 H -0.1616 0.1987 0.4481 0.050 Uiso 1 1 calc R . . C16 C -0.1211(3) 0.2257(6) 0.5549(4) 0.0409(15) Uani 1 1 d . . . H16 H -0.1573 0.1898 0.5824 0.049 Uiso 1 1 calc R . . C17 C -0.0662(4) 0.2710(6) 0.5946(4) 0.0448(17) Uani 1 1 d . . . H17 H -0.0641 0.2648 0.6495 0.054 Uiso 1 1 calc R . . C18 C -0.0137(3) 0.3257(5) 0.5560(4) 0.0393(15) Uani 1 1 d . . . H18 H 0.0238 0.3580 0.5841 0.047 Uiso 1 1 calc R . . C19 C 0.3042(3) 0.3320(4) 0.2638(3) 0.0274(11) Uani 1 1 d . . . C20 C 0.3322(3) 0.2270(5) 0.2666(3) 0.0307(12) Uani 1 1 d . . . C21 C 0.3578(3) 0.1423(5) 0.2669(3) 0.0324(13) Uani 1 1 d . . . C22 C 0.3901(3) 0.0399(4) 0.2659(3) 0.0303(12) Uani 1 1 d . . . C23 C 0.3531(3) -0.0465(5) 0.2936(5) 0.0443(16) Uani 1 1 d . . . H23 H 0.3066 -0.0385 0.3142 0.053 Uiso 1 1 calc R . . C24 C 0.3845(4) -0.1439(5) 0.2910(5) 0.054(2) Uani 1 1 d . . . H24 H 0.3596 -0.2027 0.3107 0.065 Uiso 1 1 calc R . . C25 C 0.4512(4) -0.1561(5) 0.2603(4) 0.0451(17) Uani 1 1 d . . . H25 H 0.4715 -0.2237 0.2566 0.054 Uiso 1 1 calc R . . C26 C 0.4889(3) -0.0702(5) 0.2348(4) 0.0397(14) Uani 1 1 d . . . H26 H 0.5359 -0.0783 0.2156 0.048 Uiso 1 1 calc R . . C27 C 0.4581(3) 0.0272(5) 0.2374(4) 0.0352(13) Uani 1 1 d . . . H27 H 0.4839 0.0861 0.2194 0.042 Uiso 1 1 calc R . . C28 C 0.3610(3) 0.5913(4) 0.1673(3) 0.0257(11) Uani 1 1 d . . . C29 C 0.4195(3) 0.6241(5) 0.1187(4) 0.0346(13) Uani 1 1 d . . . C30 C 0.4678(3) 0.6513(5) 0.0788(3) 0.0341(13) Uani 1 1 d . . . C31 C 0.5257(3) 0.6846(5) 0.0305(3) 0.0324(13) Uani 1 1 d . . . C32 C 0.5314(4) 0.6478(6) -0.0454(4) 0.0422(15) Uani 1 1 d . . . H32 H 0.4973 0.6004 -0.0656 0.051 Uiso 1 1 calc R . . C33 C 0.5870(4) 0.6812(6) -0.0902(4) 0.0492(18) Uani 1 1 d . . . H33 H 0.5914 0.6554 -0.1417 0.059 Uiso 1 1 calc R . . C34 C 0.6367(3) 0.7512(6) -0.0627(4) 0.0449(17) Uani 1 1 d . . . H34 H 0.6742 0.7745 -0.0952 0.054 Uiso 1 1 calc R . . C35 C 0.6313(3) 0.7872(6) 0.0131(4) 0.0412(15) Uani 1 1 d . . . H35 H 0.6658 0.8341 0.0331 0.049 Uiso 1 1 calc R . . C36 C 0.5760(3) 0.7546(5) 0.0588(4) 0.0362(14) Uani 1 1 d . . . H36 H 0.5719 0.7802 0.1104 0.043 Uiso 1 1 calc R . . C37 C 0.4146(9) 0.5838(12) 0.4484(10) 0.046(4) Uiso 0.65(5) 1 d P A 3 H37A H 0.4480 0.6409 0.4355 0.055 Uiso 0.65(5) 1 calc PR A 3 H37B H 0.4290 0.5203 0.4198 0.055 Uiso 0.65(5) 1 calc PR A 3 C38 C 0.4138(10) 0.5635(12) 0.5361(9) 0.050(4) Uiso 0.65(5) 1 d P A 3 H38A H 0.4461 0.6121 0.5634 0.059 Uiso 0.65(5) 1 calc PR A 3 H38B H 0.4286 0.4910 0.5476 0.059 Uiso 0.65(5) 1 calc PR A 3 C39 C 0.3335(11) 0.582(2) 0.5616(12) 0.076(6) Uiso 0.65(5) 1 d P A 3 H39A H 0.3082 0.5154 0.5681 0.091 Uiso 0.65(5) 1 calc PR A 3 H39B H 0.3313 0.6216 0.6111 0.091 Uiso 0.65(5) 1 calc PR A 3 C40 C 0.3023(11) 0.643(2) 0.4985(11) 0.075(5) Uiso 0.65(5) 1 d P A 3 H40A H 0.3071 0.7187 0.5086 0.090 Uiso 0.65(5) 1 calc PR A 3 H40B H 0.2513 0.6260 0.4921 0.090 Uiso 0.65(5) 1 calc PR A 3 C37A C 0.4016(18) 0.578(2) 0.467(2) 0.053(8) Uiso 0.35(5) 1 d P A 4 H37C H 0.4419 0.6249 0.4546 0.064 Uiso 0.35(5) 1 calc PR A 4 H37D H 0.4136 0.5077 0.4480 0.064 Uiso 0.35(5) 1 calc PR A 4 C38A C 0.393(2) 0.575(2) 0.5479(18) 0.054(8) Uiso 0.35(5) 1 d P A 4 H38C H 0.3932 0.5013 0.5661 0.065 Uiso 0.35(5) 1 calc PR A 4 H38D H 0.4324 0.6122 0.5739 0.065 Uiso 0.35(5) 1 calc PR A 4 C39A C 0.328(2) 0.622(5) 0.565(3) 0.101(15) Uiso 0.35(5) 1 d P A 4 H39C H 0.3315 0.6710 0.6090 0.121 Uiso 0.35(5) 1 calc PR A 4 H39D H 0.2900 0.5702 0.5750 0.121 Uiso 0.35(5) 1 calc PR A 4 C40A C 0.3165(14) 0.680(2) 0.4861(14) 0.045(7) Uiso 0.35(5) 1 d P A 4 H40C H 0.2655 0.6941 0.4773 0.054 Uiso 0.35(5) 1 calc PR A 4 H40D H 0.3427 0.7468 0.4856 0.054 Uiso 0.35(5) 1 calc PR A 4 C41 C 0.2097(7) 0.4407(13) 0.0075(7) 0.067(4) Uiso 0.65(2) 1 d PD B 1 H41A H 0.2548 0.4033 0.0178 0.081 Uiso 0.65(2) 1 calc PR B 1 H41B H 0.2194 0.5067 -0.0203 0.081 Uiso 0.65(2) 1 calc PR B 1 C42 C 0.1525(8) 0.3696(12) -0.0359(10) 0.072(5) Uiso 0.65(2) 1 d PD B 1 H42A H 0.1624 0.3663 -0.0922 0.087 Uiso 0.65(2) 1 calc PR B 1 H42B H 0.1525 0.2979 -0.0145 0.087 Uiso 0.65(2) 1 calc PR B 1 C43 C 0.0805(9) 0.4245(14) -0.0201(8) 0.064(4) Uiso 0.65(2) 1 d PD B 1 H43A H 0.0762 0.4929 -0.0462 0.076 Uiso 0.65(2) 1 calc PR B 1 H43B H 0.0389 0.3801 -0.0321 0.076 Uiso 0.65(2) 1 calc PR B 1 C44 C 0.0954(7) 0.4333(18) 0.0659(9) 0.074(7) Uiso 0.65(2) 1 d PD B 1 H44A H 0.0659 0.4893 0.0887 0.088 Uiso 0.65(2) 1 calc PR B 1 H44B H 0.0833 0.3669 0.0921 0.088 Uiso 0.65(2) 1 calc PR B 1 C41A C 0.1989(13) 0.3747(19) 0.0295(12) 0.073(9) Uiso 0.35(2) 1 d PD B 2 H41C H 0.1787 0.3059 0.0434 0.088 Uiso 0.35(2) 1 calc PR B 2 H41D H 0.2511 0.3721 0.0364 0.088 Uiso 0.35(2) 1 calc PR B 2 C42A C 0.1794(14) 0.404(3) -0.0561(13) 0.071(8) Uiso 0.35(2) 1 d PD B 2 H42C H 0.1980 0.4721 -0.0738 0.085 Uiso 0.35(2) 1 calc PR B 2 H42D H 0.1881 0.3482 -0.0947 0.085 Uiso 0.35(2) 1 calc PR B 2 C43A C 0.1032(17) 0.407(3) -0.0230(15) 0.078(11) Uiso 0.35(2) 1 d PD B 2 H43C H 0.0849 0.3347 -0.0220 0.094 Uiso 0.35(2) 1 calc PR B 2 H43D H 0.0732 0.4466 -0.0599 0.094 Uiso 0.35(2) 1 calc PR B 2 C44A C 0.0917(7) 0.455(2) 0.0604(13) 0.041(7) Uiso 0.35(2) 1 d PD B 2 H44C H 0.0705 0.5260 0.0591 0.049 Uiso 0.35(2) 1 calc PR B 2 H44D H 0.0644 0.4093 0.0956 0.049 Uiso 0.35(2) 1 calc PR B 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 0.0205(2) 0.0231(2) 0.0203(2) 0.00163(17) -0.00163(15) 0.00175(17) Mo2 0.0203(2) 0.0236(2) 0.0201(2) 0.00155(17) -0.00152(15) 0.00159(17) O1 0.0253(18) 0.0239(19) 0.0268(19) -0.0005(15) -0.0021(15) 0.0009(15) O2 0.0231(18) 0.027(2) 0.0291(19) 0.0034(16) -0.0026(15) 0.0036(15) O3 0.039(2) 0.027(2) 0.0276(19) 0.0053(16) 0.0075(16) 0.0026(17) O4 0.0215(18) 0.028(2) 0.034(2) 0.0025(17) 0.0021(15) 0.0012(15) O5 0.0241(18) 0.028(2) 0.032(2) 0.0021(16) -0.0056(15) 0.0034(16) O6 0.0274(19) 0.024(2) 0.0286(19) 0.0003(16) -0.0003(15) 0.0044(15) O7 0.0219(18) 0.030(2) 0.0301(19) 0.0010(16) 0.0000(15) 0.0013(15) O8 0.033(2) 0.030(2) 0.029(2) 0.0028(17) 0.0084(16) 0.0006(17) O9 0.068(4) 0.104(5) 0.053(3) -0.040(3) -0.034(3) 0.033(4) O10 0.061(3) 0.091(4) 0.034(3) -0.023(3) -0.015(2) 0.021(3) C1 0.021(2) 0.030(3) 0.031(3) 0.002(2) 0.004(2) 0.002(2) C2 0.027(3) 0.030(3) 0.034(3) 0.003(2) 0.001(2) 0.001(2) C3 0.026(3) 0.032(3) 0.036(3) 0.003(2) -0.001(2) -0.001(2) C4 0.028(3) 0.025(3) 0.035(3) -0.001(2) -0.003(2) 0.001(2) C5 0.028(3) 0.035(3) 0.061(4) 0.000(3) 0.002(3) -0.004(3) C6 0.042(4) 0.026(3) 0.070(5) 0.009(3) -0.011(3) -0.006(3) C7 0.039(3) 0.031(3) 0.047(4) -0.001(3) -0.011(3) 0.007(3) C8 0.030(3) 0.033(3) 0.055(4) -0.001(3) -0.001(3) 0.007(3) C9 0.028(3) 0.029(3) 0.046(3) 0.002(3) 0.001(2) -0.002(2) C10 0.024(3) 0.021(3) 0.033(3) 0.005(2) 0.006(2) 0.003(2) C11 0.033(3) 0.037(3) 0.039(3) 0.004(3) 0.009(3) -0.001(3) C12 0.037(3) 0.038(3) 0.035(3) 0.004(3) 0.005(3) 0.003(3) C13 0.032(3) 0.033(3) 0.031(3) 0.000(2) 0.007(2) 0.001(2) C14 0.033(3) 0.053(4) 0.030(3) 0.000(3) 0.007(2) 0.002(3) C15 0.034(3) 0.054(4) 0.037(3) -0.008(3) -0.001(3) -0.005(3) C16 0.037(3) 0.052(4) 0.033(3) -0.001(3) 0.011(3) -0.014(3) C17 0.044(4) 0.064(5) 0.027(3) -0.002(3) 0.007(3) -0.015(3) C18 0.037(3) 0.047(4) 0.034(3) -0.003(3) -0.001(3) -0.012(3) C19 0.021(2) 0.028(3) 0.033(3) 0.004(2) 0.003(2) 0.002(2) C20 0.027(3) 0.031(3) 0.034(3) 0.003(2) 0.000(2) 0.002(2) C21 0.028(3) 0.034(3) 0.035(3) 0.002(2) -0.002(2) 0.001(2) C22 0.027(3) 0.024(3) 0.041(3) -0.002(2) -0.005(2) 0.001(2) C23 0.027(3) 0.033(3) 0.072(5) 0.003(3) 0.003(3) 0.001(3) C24 0.044(4) 0.026(3) 0.091(6) 0.009(4) -0.011(4) -0.006(3) C25 0.044(4) 0.026(3) 0.065(5) -0.005(3) -0.017(3) 0.006(3) C26 0.034(3) 0.039(4) 0.047(4) -0.008(3) -0.001(3) 0.009(3) C27 0.028(3) 0.032(3) 0.046(3) -0.002(3) -0.001(2) -0.002(2) C28 0.024(3) 0.025(3) 0.027(3) 0.003(2) 0.001(2) 0.001(2) C29 0.027(3) 0.040(3) 0.036(3) 0.001(3) 0.002(2) -0.003(2) C30 0.032(3) 0.037(3) 0.033(3) 0.002(3) 0.005(2) 0.001(3) C31 0.027(3) 0.039(3) 0.031(3) 0.003(3) 0.006(2) 0.002(2) C32 0.041(3) 0.047(4) 0.038(3) -0.004(3) 0.006(3) -0.012(3) C33 0.046(4) 0.069(5) 0.033(3) -0.012(3) 0.011(3) -0.016(4) C34 0.036(3) 0.063(5) 0.035(3) 0.001(3) 0.009(3) -0.015(3) C35 0.034(3) 0.051(4) 0.039(3) -0.005(3) 0.001(3) -0.009(3) C36 0.033(3) 0.046(4) 0.030(3) -0.002(3) 0.004(2) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O7 2.094(4) . ? Mo1 O3 2.100(4) . ? Mo1 O5 2.101(4) . ? Mo1 O1 2.107(4) . ? Mo1 Mo2 2.1106(6) . ? Mo2 O4 2.092(4) . ? Mo2 O2 2.101(4) . ? Mo2 O8 2.114(4) . ? Mo2 O6 2.117(4) . ? O1 C1 1.266(6) . ? O2 C1 1.270(7) . ? O3 C10 1.292(7) . ? O4 C10 1.272(7) . ? O5 C19 1.277(7) . ? O6 C19 1.273(6) . ? O7 C28 1.278(6) . ? O8 C28 1.277(7) . ? O9 C37A 1.35(3) . ? O9 C40A 1.40(2) . ? O9 C37 1.435(16) . ? O9 C40 1.469(19) . ? O10 C44 1.412(12) . ? O10 C41 1.442(11) . ? O10 C41A 1.447(15) . ? O10 C44A 1.467(13) . ? C1 C2 1.449(8) . ? C2 C3 1.195(8) . ? C3 C4 1.437(8) . ? C4 C9 1.388(8) . ? C4 C5 1.395(8) . ? C5 C6 1.380(9) . ? C6 C7 1.375(9) . ? C7 C8 1.366(9) . ? C8 C9 1.382(8) . ? C10 C11 1.452(8) . ? C11 C12 1.202(8) . ? C12 C13 1.425(8) . ? C13 C18 1.399(8) . ? C13 C14 1.406(9) . ? C14 C15 1.375(9) . ? C15 C16 1.373(9) . ? C16 C17 1.369(9) . ? C17 C18 1.382(9) . ? C19 C20 1.448(8) . ? C20 C21 1.189(8) . ? C21 C22 1.447(8) . ? C22 C27 1.380(8) . ? C22 C23 1.393(9) . ? C23 C24 1.382(9) . ? C24 C25 1.371(10) . ? C25 C26 1.383(10) . ? C26 C27 1.378(9) . ? C28 C29 1.444(8) . ? C29 C30 1.192(8) . ? C30 C31 1.436(8) . ? C31 C36 1.393(9) . ? C31 C32 1.395(9) . ? C32 C33 1.369(9) . ? C33 C34 1.381(9) . ? C34 C35 1.388(9) . ? C35 C36 1.371(8) . ? C37 C38 1.53(2) . ? C38 C39 1.59(2) . ? C39 C40 1.46(3) . ? C37A C38A 1.40(4) . ? C38A C39A 1.40(5) . ? C39A C40A 1.56(5) . ? C41 C42 1.597(14) . ? C42 C43 1.550(19) . ? C43 C44 1.511(14) . ? C41A C42A 1.565(17) . ? C42A C43A 1.54(2) . ? C43A C44A 1.580(17) . ? 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 O7 Mo1 O3 175.87(15) . . ? O7 Mo1 O5 90.05(15) . . ? O3 Mo1 O5 88.99(15) . . ? O7 Mo1 O1 89.58(15) . . ? O3 Mo1 O1 91.16(15) . . ? O5 Mo1 O1 176.82(15) . . ? O7 Mo1 Mo2 92.28(10) . . ? O3 Mo1 Mo2 91.77(11) . . ? O5 Mo1 Mo2 92.13(10) . . ? O1 Mo1 Mo2 91.04(10) . . ? O4 Mo2 O2 90.43(15) . . ? O4 Mo2 Mo1 92.25(11) . . ? O2 Mo2 Mo1 92.22(10) . . ? O4 Mo2 O8 176.21(15) . . ? O2 Mo2 O8 89.47(15) . . ? Mo1 Mo2 O8 91.55(11) . . ? O4 Mo2 O6 89.48(15) . . ? O2 Mo2 O6 176.45(15) . . ? Mo1 Mo2 O6 91.33(10) . . ? O8 Mo2 O6 90.38(15) . . ? C1 O1 Mo1 117.3(4) . . ? C1 O2 Mo2 116.3(3) . . ? C10 O3 Mo1 116.0(3) . . ? C10 O4 Mo2 116.4(3) . . ? C19 O5 Mo1 116.9(3) . . ? C19 O6 Mo2 116.9(4) . . ? C28 O7 Mo1 116.5(3) . . ? C28 O8 Mo2 116.2(3) . . ? C37A O9 C40A 98.9(17) . . ? C40A O9 C37 109.5(13) . . ? C37A O9 C40 97.0(18) . . ? C37 O9 C40 111.9(11) . . ? C44 O10 C41 112.7(9) . . ? C44 O10 C41A 99.3(15) . . ? C41 O10 C44A 111.8(10) . . ? C41A O10 C44A 106.2(12) . . ? O1 C1 O2 123.1(5) . . ? O1 C1 C2 118.6(5) . . ? O2 C1 C2 118.3(5) . . ? C3 C2 C1 176.6(6) . . ? C2 C3 C4 177.7(7) . . ? C9 C4 C5 119.3(5) . . ? C9 C4 C3 119.7(5) . . ? C5 C4 C3 121.0(5) . . ? C6 C5 C4 119.7(6) . . ? C7 C6 C5 120.6(6) . . ? C8 C7 C6 119.7(6) . . ? C7 C8 C9 120.9(6) . . ? C8 C9 C4 119.7(6) . . ? O4 C10 O3 123.5(5) . . ? O4 C10 C11 118.4(5) . . ? O3 C10 C11 118.1(5) . . ? C12 C11 C10 174.4(7) . . ? C11 C12 C13 178.8(7) . . ? C18 C13 C14 119.4(5) . . ? C18 C13 C12 121.1(6) . . ? C14 C13 C12 119.5(5) . . ? C15 C14 C13 119.6(6) . . ? C16 C15 C14 120.6(6) . . ? C17 C16 C15 120.2(6) . . ? C16 C17 C18 120.9(6) . . ? C17 C18 C13 119.2(6) . . ? O6 C19 O5 122.7(5) . . ? O6 C19 C20 118.2(5) . . ? O5 C19 C20 119.0(5) . . ? C21 C20 C19 177.0(6) . . ? C20 C21 C22 178.7(7) . . ? C27 C22 C23 119.4(6) . . ? C27 C22 C21 120.0(5) . . ? C23 C22 C21 120.6(5) . . ? C24 C23 C22 119.7(6) . . ? C25 C24 C23 120.4(7) . . ? C24 C25 C26 120.1(6) . . ? C27 C26 C25 119.8(6) . . ? C26 C27 C22 120.6(6) . . ? O8 C28 O7 123.5(5) . . ? O8 C28 C29 117.8(5) . . ? O7 C28 C29 118.7(5) . . ? C30 C29 C28 179.8(8) . . ? C29 C30 C31 179.6(8) . . ? C36 C31 C32 119.6(5) . . ? C36 C31 C30 120.3(5) . . ? C32 C31 C30 120.1(6) . . ? C33 C32 C31 118.8(6) . . ? C32 C33 C34 121.8(6) . . ? C33 C34 C35 119.3(6) . . ? C36 C35 C34 119.7(6) . . ? C35 C36 C31 120.7(6) . . ? O9 C37 C38 105.0(11) . . ? C37 C38 C39 104.8(12) . . ? C40 C39 C38 104.9(15) . . ? C39 C40 O9 104.7(14) . . ? O9 C37A C38A 113(2) . . ? C39A C38A C37A 107(3) . . ? C38A C39A C40A 98(3) . . ? O9 C40A C39A 105(2) . . ? O10 C41 C42 95.7(10) . . ? C43 C42 C41 104.3(12) . . ? C44 C43 C42 92.5(13) . . ? O10 C44 C43 109.0(12) . . ? O10 C41A C42A 105.4(16) . . ? C43A C42A C41A 83(2) . . ? C42A C43A C44A 118(2) . . ? O10 C44A C43A 92.5(16) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.154 _refine_diff_density_min -1.493 _refine_diff_density_rms 0.120 #===END