# 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_email chmzhaoj@nus.edu.sg loop_ _publ_author_name 'Shenyu Li.' 'Zhe Wang.' 'Andy Hor' 'Jin Zhao.' data_9182 _database_code_depnum_ccdc_archive 'CCDC 824843' #TrackingRef '9182.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H42 Mo8 N4 O23' _chemical_formula_weight 1762.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.8862(5) _cell_length_b 8.4404(4) _cell_length_c 31.7569(17) _cell_angle_alpha 90.00 _cell_angle_beta 94.4590(10) _cell_angle_gamma 90.00 _cell_volume 2641.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5184 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.50 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 2.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1708 _exptl_absorpt_coefficient_mu 1.920 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5139 _exptl_absorpt_correction_T_max 0.8312 _exptl_absorpt_process_details 'Sadabs,(Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 18240 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6056 _reflns_number_gt 5315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+3.4522P] 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 6056 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 0.04604(4) 1.04436(4) 0.619419(12) 0.02983(9) Uani 1 1 d . . . Mo2 Mo 0.53446(4) 0.35562(4) 0.562009(12) 0.03169(10) Uani 1 1 d . . . Mo3 Mo 0.27958(3) 0.55357(4) 0.515549(12) 0.02870(9) Uani 1 1 d . . . Mo4 Mo 0.42498(3) 0.27202(4) 0.464571(12) 0.02929(9) Uani 1 1 d . . . N1 N 0.2982(3) 0.8148(4) 0.63708(10) 0.0285(7) Uani 1 1 d . . . N2 N 0.1137(4) 0.6795(4) 0.63292(11) 0.0321(8) Uani 1 1 d . . . O1 O 0.1428(4) 1.1796(4) 0.64842(11) 0.0527(9) Uani 1 1 d . . . O2 O -0.0910(4) 0.9965(5) 0.64564(12) 0.0592(10) Uani 1 1 d . . . O3 O 0.7034(3) 0.3385(3) 0.53826(10) 0.0351(7) Uani 1 1 d . . . O4 O 0.5533(4) 0.2498(4) 0.60697(10) 0.0489(9) Uani 1 1 d . . . O5 O 0.5811(3) 0.5660(3) 0.57972(9) 0.0326(6) Uani 1 1 d . . . O6 O 0.3802(3) 0.7277(3) 0.54089(9) 0.0319(6) Uani 1 1 d . . . O7 O 0.1193(3) 0.5942(3) 0.52662(11) 0.0410(8) Uani 1 1 d . . . O8 O 0.3708(3) 0.1100(3) 0.43740(10) 0.0390(7) Uani 1 1 d . . . O9 O 0.3450(3) 0.4249(3) 0.56127(9) 0.0313(6) Uani 1 1 d . . . O10 O 0.2603(3) 0.3628(3) 0.48137(9) 0.0290(6) Uani 1 1 d . . . O11 O 0.4632(3) 0.1990(3) 0.52082(9) 0.0320(6) Uani 1 1 d . . . O12 O 0.5000 0.5000 0.5000 0.0227(7) Uani 1 2 d S . . C1 C 0.1627(4) 0.8285(4) 0.63122(12) 0.0276(8) Uani 1 1 d . . . C2 C 0.3337(5) 0.6569(5) 0.64160(13) 0.0346(9) Uani 1 1 d . . . H2 H 0.4221 0.6159 0.6457 0.041 Uiso 1 1 calc R . . C3 C 0.2185(5) 0.5735(5) 0.63899(13) 0.0369(10) Uani 1 1 d . . . H3 H 0.2108 0.4628 0.6409 0.044 Uiso 1 1 calc R . . C4 C 0.3991(4) 0.9443(5) 0.63614(14) 0.0347(9) Uani 1 1 d . . . H4A H 0.3518 1.0460 0.6325 0.042 Uiso 1 1 calc R . . H4B H 0.4536 0.9292 0.6119 0.042 Uiso 1 1 calc R . . C5 C 0.4915(4) 0.9481(5) 0.67627(15) 0.0363(10) Uani 1 1 d . . . C6 C 0.6165(5) 0.8748(6) 0.67870(16) 0.0473(12) Uani 1 1 d . . . H6 H 0.6466 0.8251 0.6546 0.057 Uiso 1 1 calc R . . C7 C 0.6981(6) 0.8737(7) 0.71604(18) 0.0601(15) Uani 1 1 d . . . H7 H 0.7826 0.8219 0.7174 0.072 Uiso 1 1 calc R . . C8 C 0.6567(6) 0.9469(8) 0.75057(19) 0.0701(18) Uani 1 1 d . . . H8 H 0.7115 0.9434 0.7761 0.084 Uiso 1 1 calc R . . C9 C 0.5346(7) 1.0267(9) 0.7488(2) 0.078(2) Uani 1 1 d . . . H9 H 0.5079 1.0813 0.7726 0.094 Uiso 1 1 calc R . . C10 C 0.4519(5) 1.0255(7) 0.71145(18) 0.0598(15) Uani 1 1 d . . . H10 H 0.3679 1.0782 0.7101 0.072 Uiso 1 1 calc R . . C11 C -0.0288(5) 0.6306(5) 0.62755(15) 0.0398(10) Uani 1 1 d . . . H11A H -0.0424 0.5659 0.6020 0.048 Uiso 1 1 calc R . . H11B H -0.0857 0.7253 0.6234 0.048 Uiso 1 1 calc R . . C12 C -0.0751(4) 0.5376(5) 0.66439(14) 0.0342(9) Uani 1 1 d . . . C13 C -0.0264(6) 0.5697(6) 0.70539(16) 0.0510(13) Uani 1 1 d . . . H13 H 0.0411 0.6470 0.7109 0.061 Uiso 1 1 calc R . . C14 C -0.0775(7) 0.4874(8) 0.73858(18) 0.0707(18) Uani 1 1 d . . . H14 H -0.0441 0.5087 0.7665 0.085 Uiso 1 1 calc R . . C15 C -0.1760(6) 0.3759(9) 0.7306(2) 0.079(2) Uani 1 1 d . . . H15 H -0.2120 0.3223 0.7532 0.094 Uiso 1 1 calc R . . C16 C -0.2222(6) 0.3420(8) 0.6905(2) 0.0705(18) Uani 1 1 d . . . H16 H -0.2892 0.2639 0.6854 0.085 Uiso 1 1 calc R . . C17 C -0.1720(5) 0.4210(6) 0.65655(18) 0.0499(12) Uani 1 1 d . . . H17 H -0.2035 0.3955 0.6287 0.060 Uiso 1 1 calc R . . C18 C -0.0210(4) 0.9333(5) 0.54964(13) 0.0331(9) Uani 1 1 d . . . H18 H -0.0605 0.8269 0.5440 0.040 Uiso 1 1 calc R . . C19 C -0.0926(4) 1.0700(5) 0.55451(15) 0.0381(10) Uani 1 1 d . . . H19 H -0.1927 1.0804 0.5517 0.046 Uiso 1 1 calc R . . C20 C 0.0022(5) 1.1978(5) 0.55893(14) 0.0395(10) Uani 1 1 d . . . H20 H -0.0215 1.3117 0.5585 0.047 Uiso 1 1 calc R . . C21 C 0.1318(4) 1.1359(5) 0.55435(14) 0.0379(10) Uani 1 1 d . . . H21 H 0.2155 1.1985 0.5520 0.045 Uiso 1 1 calc R . . C22 C 0.1201(4) 0.9732(5) 0.54994(13) 0.0346(9) Uani 1 1 d . . . H22 H 0.1946 0.8992 0.5446 0.041 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 0.02901(19) 0.02724(18) 0.0337(2) -0.00008(15) 0.00534(15) 0.00094(14) Mo2 0.02896(19) 0.03253(19) 0.0331(2) 0.00925(15) -0.00053(15) -0.00229(14) Mo3 0.01893(17) 0.02662(17) 0.0410(2) -0.00149(15) 0.00524(14) 0.00105(13) Mo4 0.02579(18) 0.02457(17) 0.0378(2) -0.00684(15) 0.00441(15) -0.00434(13) N1 0.0290(17) 0.0284(16) 0.0277(18) 0.0016(14) 0.0005(14) -0.0015(13) N2 0.038(2) 0.0300(17) 0.0273(18) 0.0049(14) -0.0025(15) -0.0053(15) O1 0.058(2) 0.0429(18) 0.056(2) -0.0164(17) 0.0008(18) -0.0062(16) O2 0.047(2) 0.075(2) 0.059(2) -0.001(2) 0.0247(18) -0.0061(19) O3 0.0256(15) 0.0351(15) 0.0439(18) 0.0065(14) -0.0010(13) 0.0059(12) O4 0.056(2) 0.0486(19) 0.0409(19) 0.0181(16) -0.0071(16) -0.0123(16) O5 0.0330(16) 0.0344(15) 0.0305(15) 0.0016(13) 0.0022(12) -0.0083(12) O6 0.0239(14) 0.0281(14) 0.0447(17) -0.0076(13) 0.0095(13) -0.0001(11) O7 0.0217(14) 0.0364(16) 0.066(2) -0.0109(16) 0.0092(14) 0.0016(12) O8 0.0348(16) 0.0320(15) 0.0510(19) -0.0128(14) 0.0090(14) -0.0098(13) O9 0.0307(15) 0.0298(14) 0.0345(16) 0.0018(12) 0.0086(12) -0.0048(12) O10 0.0204(13) 0.0280(14) 0.0389(16) -0.0056(12) 0.0043(12) -0.0029(11) O11 0.0318(15) 0.0216(13) 0.0422(17) 0.0030(12) 0.0007(13) -0.0017(11) O12 0.0181(17) 0.0236(17) 0.0263(19) -0.0008(15) 0.0021(15) 0.0001(14) C1 0.030(2) 0.0275(19) 0.025(2) 0.0009(16) 0.0017(16) -0.0050(16) C2 0.038(2) 0.037(2) 0.029(2) 0.0065(18) 0.0000(18) 0.0077(19) C3 0.056(3) 0.025(2) 0.030(2) 0.0004(17) 0.000(2) 0.0021(19) C4 0.028(2) 0.036(2) 0.040(2) 0.0020(19) 0.0049(18) -0.0034(17) C5 0.026(2) 0.043(2) 0.040(2) 0.002(2) 0.0041(18) -0.0075(18) C6 0.035(3) 0.067(3) 0.040(3) -0.002(2) 0.006(2) 0.003(2) C7 0.041(3) 0.080(4) 0.058(4) 0.004(3) -0.009(3) 0.003(3) C8 0.053(4) 0.108(5) 0.047(3) -0.010(3) -0.012(3) -0.016(3) C9 0.069(4) 0.115(6) 0.050(3) -0.033(4) -0.001(3) -0.001(4) C10 0.040(3) 0.084(4) 0.055(3) -0.027(3) 0.001(2) 0.003(3) C11 0.044(3) 0.033(2) 0.040(3) 0.006(2) -0.008(2) -0.0121(19) C12 0.034(2) 0.026(2) 0.042(2) 0.0063(18) -0.0007(19) 0.0007(17) C13 0.052(3) 0.059(3) 0.041(3) -0.001(3) 0.002(2) -0.004(2) C14 0.068(4) 0.107(5) 0.038(3) 0.017(3) 0.005(3) 0.007(4) C15 0.046(3) 0.106(5) 0.086(5) 0.053(4) 0.019(3) 0.011(3) C16 0.044(3) 0.080(4) 0.087(5) 0.033(4) 0.004(3) -0.011(3) C17 0.041(3) 0.051(3) 0.057(3) 0.009(3) -0.003(2) -0.010(2) C18 0.041(2) 0.028(2) 0.029(2) 0.0054(17) -0.0076(18) -0.0046(18) C19 0.029(2) 0.039(2) 0.045(3) 0.011(2) -0.0053(19) 0.0008(18) C20 0.053(3) 0.026(2) 0.038(3) 0.0065(18) -0.005(2) 0.0030(19) C21 0.036(2) 0.042(2) 0.035(2) 0.014(2) 0.0003(19) -0.0115(19) C22 0.036(2) 0.043(2) 0.026(2) 0.0047(18) 0.0041(18) 0.0102(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O2 1.694(3) . ? Mo1 O1 1.711(3) . ? Mo1 C1 2.173(4) . ? Mo1 C20 2.329(4) . ? Mo1 C19 2.395(4) . ? Mo1 C21 2.420(4) . ? Mo1 C18 2.450(4) . ? Mo1 C22 2.453(4) . ? Mo2 O4 1.682(3) . ? Mo2 O3 1.891(3) . ? Mo2 O5 1.908(3) . ? Mo2 O11 1.952(3) . ? Mo2 O9 1.960(3) . ? Mo2 O12 2.3183(4) . ? Mo3 O7 1.685(3) . ? Mo3 O9 1.887(3) . ? Mo3 O6 1.916(3) . ? Mo3 O10 1.943(3) . ? Mo3 O3 1.955(3) 3_666 ? Mo3 O12 2.3160(3) . ? Mo4 O8 1.682(3) . ? Mo4 O11 1.899(3) . ? Mo4 O10 1.912(3) . ? Mo4 O6 1.947(3) 3_666 ? Mo4 O5 1.959(3) 3_666 ? Mo4 O12 2.3214(3) . ? N1 C1 1.343(5) . ? N1 C2 1.383(5) . ? N1 C4 1.481(5) . ? N2 C1 1.350(5) . ? N2 C3 1.372(5) . ? N2 C11 1.465(5) . ? O3 Mo3 1.955(3) 3_666 ? O5 Mo4 1.959(3) 3_666 ? O6 Mo4 1.947(3) 3_666 ? O12 Mo3 2.3161(3) 3_666 ? O12 Mo2 2.3184(4) 3_666 ? O12 Mo4 2.3213(3) 3_666 ? C2 C3 1.336(6) . ? C4 C5 1.509(6) . ? C5 C10 1.377(7) . ? C5 C6 1.379(6) . ? C6 C7 1.381(7) . ? C7 C8 1.350(8) . ? C8 C9 1.379(9) . ? C9 C10 1.387(8) . ? C11 C12 1.510(6) . ? C12 C13 1.379(7) . ? C12 C17 1.382(6) . ? C13 C14 1.390(7) . ? C14 C15 1.364(9) . ? C15 C16 1.352(10) . ? C16 C17 1.390(8) . ? C18 C19 1.369(6) . ? C18 C22 1.435(6) . ? C19 C20 1.428(6) . ? C20 C21 1.401(6) . ? C21 C22 1.384(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mo1 O1 109.23(18) . . ? O2 Mo1 C1 98.59(17) . . ? O1 Mo1 C1 101.51(16) . . ? O2 Mo1 C20 115.69(18) . . ? O1 Mo1 C20 97.67(17) . . ? C1 Mo1 C20 132.10(16) . . ? O2 Mo1 C19 91.05(18) . . ? O1 Mo1 C19 131.40(16) . . ? C1 Mo1 C19 119.01(15) . . ? C20 Mo1 C19 35.16(15) . . ? O2 Mo1 C21 147.41(18) . . ? O1 Mo1 C21 91.64(16) . . ? C1 Mo1 C21 101.45(15) . . ? C20 Mo1 C21 34.25(15) . . ? C19 Mo1 C21 56.72(15) . . ? O2 Mo1 C18 100.54(17) . . ? O1 Mo1 C18 147.43(16) . . ? C1 Mo1 C18 86.43(14) . . ? C20 Mo1 C18 56.41(15) . . ? C19 Mo1 C18 32.81(14) . . ? C21 Mo1 C18 55.80(14) . . ? O2 Mo1 C22 133.64(17) . . ? O1 Mo1 C22 117.00(16) . . ? C1 Mo1 C22 76.01(14) . . ? C20 Mo1 C22 56.19(15) . . ? C19 Mo1 C22 55.87(15) . . ? C21 Mo1 C22 32.99(15) . . ? C18 Mo1 C22 34.03(14) . . ? O4 Mo2 O3 104.76(15) . . ? O4 Mo2 O5 103.62(14) . . ? O3 Mo2 O5 89.31(12) . . ? O4 Mo2 O11 102.69(14) . . ? O3 Mo2 O11 88.01(12) . . ? O5 Mo2 O11 153.35(12) . . ? O4 Mo2 O9 102.20(15) . . ? O3 Mo2 O9 152.97(12) . . ? O5 Mo2 O9 86.25(12) . . ? O11 Mo2 O9 84.20(12) . . ? O4 Mo2 O12 177.92(12) . . ? O3 Mo2 O12 77.14(9) . . ? O5 Mo2 O12 77.14(8) . . ? O11 Mo2 O12 76.42(8) . . ? O9 Mo2 O12 75.87(8) . . ? O7 Mo3 O9 103.19(14) . . ? O7 Mo3 O6 102.86(13) . . ? O9 Mo3 O6 89.00(12) . . ? O7 Mo3 O10 103.43(13) . . ? O9 Mo3 O10 88.04(12) . . ? O6 Mo3 O10 153.53(11) . . ? O7 Mo3 O3 103.52(14) . 3_666 ? O9 Mo3 O3 153.27(11) . 3_666 ? O6 Mo3 O3 86.15(13) . 3_666 ? O10 Mo3 O3 84.77(12) . 3_666 ? O7 Mo3 O12 179.47(12) . . ? O9 Mo3 O12 77.28(8) . . ? O6 Mo3 O12 76.87(8) . . ? O10 Mo3 O12 76.82(8) . . ? O3 Mo3 O12 76.02(8) 3_666 . ? O8 Mo4 O11 104.52(14) . . ? O8 Mo4 O10 103.01(13) . . ? O11 Mo4 O10 88.79(12) . . ? O8 Mo4 O6 103.47(13) . 3_666 ? O11 Mo4 O6 87.63(12) . 3_666 ? O10 Mo4 O6 153.33(11) . 3_666 ? O8 Mo4 O5 102.03(14) . 3_666 ? O11 Mo4 O5 153.41(11) . 3_666 ? O10 Mo4 O5 86.64(12) . 3_666 ? O6 Mo4 O5 84.84(12) 3_666 3_666 ? O8 Mo4 O12 178.14(11) . . ? O11 Mo4 O12 77.31(8) . . ? O10 Mo4 O12 77.25(8) . . ? O6 Mo4 O12 76.18(8) 3_666 . ? O5 Mo4 O12 76.12(8) 3_666 . ? C1 N1 C2 109.8(3) . . ? C1 N1 C4 126.9(3) . . ? C2 N1 C4 123.2(3) . . ? C1 N2 C3 110.1(4) . . ? C1 N2 C11 127.0(4) . . ? C3 N2 C11 122.8(4) . . ? Mo2 O3 Mo3 116.85(14) . 3_666 ? Mo2 O5 Mo4 116.40(14) . 3_666 ? Mo3 O6 Mo4 116.65(13) . 3_666 ? Mo3 O9 Mo2 116.80(13) . . ? Mo4 O10 Mo3 116.07(13) . . ? Mo4 O11 Mo2 116.46(13) . . ? Mo3 O12 Mo3 179.999(4) . 3_666 ? Mo3 O12 Mo2 90.006(13) . . ? Mo3 O12 Mo2 89.995(13) 3_666 . ? Mo3 O12 Mo2 89.996(13) . 3_666 ? Mo3 O12 Mo2 90.004(13) 3_666 3_666 ? Mo2 O12 Mo2 180.0 . 3_666 ? Mo3 O12 Mo4 90.302(12) . 3_666 ? Mo3 O12 Mo4 89.699(12) 3_666 3_666 ? Mo2 O12 Mo4 90.211(14) . 3_666 ? Mo2 O12 Mo4 89.790(14) 3_666 3_666 ? Mo3 O12 Mo4 89.698(12) . . ? Mo3 O12 Mo4 90.302(12) 3_666 . ? Mo2 O12 Mo4 89.788(14) . . ? Mo2 O12 Mo4 90.210(14) 3_666 . ? Mo4 O12 Mo4 179.999(16) 3_666 . ? N1 C1 N2 105.8(3) . . ? N1 C1 Mo1 127.3(3) . . ? N2 C1 Mo1 126.9(3) . . ? C3 C2 N1 107.1(4) . . ? C2 C3 N2 107.2(4) . . ? N1 C4 C5 111.3(3) . . ? C10 C5 C6 118.5(5) . . ? C10 C5 C4 120.3(4) . . ? C6 C5 C4 121.2(4) . . ? C5 C6 C7 120.8(5) . . ? C8 C7 C6 120.0(5) . . ? C7 C8 C9 120.7(6) . . ? C8 C9 C10 119.2(6) . . ? C5 C10 C9 120.8(5) . . ? N2 C11 C12 113.8(4) . . ? C13 C12 C17 119.7(5) . . ? C13 C12 C11 121.6(4) . . ? C17 C12 C11 118.6(4) . . ? C12 C13 C14 119.8(5) . . ? C15 C14 C13 120.1(6) . . ? C16 C15 C14 120.2(6) . . ? C15 C16 C17 121.0(6) . . ? C12 C17 C16 119.1(5) . . ? C19 C18 C22 108.2(4) . . ? C19 C18 Mo1 71.4(3) . . ? C22 C18 Mo1 73.1(2) . . ? C18 C19 C20 107.8(4) . . ? C18 C19 Mo1 75.8(3) . . ? C20 C19 Mo1 69.9(2) . . ? C21 C20 C19 107.9(4) . . ? C21 C20 Mo1 76.4(2) . . ? C19 C20 Mo1 74.9(2) . . ? C22 C21 C20 108.1(4) . . ? C22 C21 Mo1 74.8(2) . . ? C20 C21 Mo1 69.3(2) . . ? C21 C22 C18 107.9(4) . . ? C21 C22 Mo1 72.2(3) . . ? C18 C22 Mo1 72.9(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.668 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.110 # Attachment '9589.cif' data_9589 _database_code_depnum_ccdc_archive 'CCDC 824844' #TrackingRef '9589.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H53 Mo6 N5 O19' _chemical_formula_weight 1531.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7001(5) _cell_length_b 15.3922(7) _cell_length_c 15.8533(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.2250(10) _cell_angle_gamma 90.00 _cell_volume 2595.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7323 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.48 _exptl_crystal_description Rod _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.960 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 1.484 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5614 _exptl_absorpt_correction_T_max 0.8905 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _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 '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 17932 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5957 _reflns_number_gt 5344 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+3.2796P] 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 5957 _refine_ls_number_parameters 355 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _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 0.56689(3) 0.363337(17) 0.544662(18) 0.01464(8) Uani 1 1 d . . . Mo2 Mo 0.66487(3) 0.562282(18) 0.586984(18) 0.01645(8) Uani 1 1 d . . . Mo3 Mo 0.62599(3) 0.492879(18) 0.389638(18) 0.01680(8) Uani 1 1 d . . . O1 O 0.4274(2) 0.33836(14) 0.46223(14) 0.0142(4) Uani 1 1 d . . . O2 O 0.6210(2) 0.26446(15) 0.57690(15) 0.0191(5) Uani 1 1 d . . . O3 O 0.4539(2) 0.39219(14) 0.62311(14) 0.0148(4) Uani 1 1 d . . . O4 O 0.5288(2) 0.55278(15) 0.65959(14) 0.0168(5) Uani 1 1 d . . . O5 O 0.7824(2) 0.60870(16) 0.65086(16) 0.0231(5) Uani 1 1 d . . . O6 O 0.7188(2) 0.48987(16) 0.31041(16) 0.0234(5) Uani 1 1 d . . . O7 O 0.6901(2) 0.44009(14) 0.60579(14) 0.0161(5) Uani 1 1 d . . . O8 O 0.6624(2) 0.38668(14) 0.44682(14) 0.0158(5) Uani 1 1 d . . . O9 O 0.7320(2) 0.54902(14) 0.48200(14) 0.0157(5) Uani 1 1 d . . . O10 O 0.5000 0.5000 0.5000 0.0118(6) Uani 1 2 d S . . N1 N 0.7998(2) 0.29335(18) 0.77358(17) 0.0157(5) Uani 1 1 d . . . N2 N 0.9284(3) 0.22469(18) 0.70120(18) 0.0171(6) Uani 1 1 d . . . C1 C 0.8542(3) 0.2932(2) 0.7019(2) 0.0154(6) Uani 1 1 d . . . H1 H 0.8416 0.3357 0.6583 0.018 Uiso 1 1 calc R . . C2 C 0.8415(4) 0.2216(2) 0.8207(2) 0.0289(9) Uani 1 1 d . . . H2 H 0.8180 0.2054 0.8746 0.035 Uiso 1 1 calc R . . C3 C 0.9224(4) 0.1785(3) 0.7756(3) 0.0302(9) Uani 1 1 d . . . H3 H 0.9665 0.1266 0.7918 0.036 Uiso 1 1 calc R . . C4 C 0.7197(3) 0.3620(2) 0.8007(2) 0.0163(6) Uani 1 1 d . . . C5 C 0.5950(3) 0.3432(2) 0.8094(2) 0.0172(6) Uani 1 1 d . . . C6 C 0.5224(3) 0.4107(2) 0.8363(2) 0.0196(7) Uani 1 1 d . . . H6 H 0.4369 0.3996 0.8434 0.024 Uiso 1 1 calc R . . C7 C 0.5698(4) 0.4932(2) 0.8531(2) 0.0218(7) Uani 1 1 d . . . C8 C 0.6949(3) 0.5088(2) 0.8419(2) 0.0201(7) Uani 1 1 d . . . H8 H 0.7282 0.5654 0.8530 0.024 Uiso 1 1 calc R . . C9 C 0.7735(3) 0.4440(2) 0.8150(2) 0.0175(7) Uani 1 1 d . . . C10 C 0.5372(3) 0.2556(2) 0.7876(2) 0.0216(7) Uani 1 1 d . . . H10A H 0.4467 0.2623 0.7716 0.032 Uiso 1 1 calc R . . H10B H 0.5513 0.2171 0.8370 0.032 Uiso 1 1 calc R . . H10C H 0.5761 0.2303 0.7401 0.032 Uiso 1 1 calc R . . C11 C 0.4881(4) 0.5651(3) 0.8800(2) 0.0296(9) Uani 1 1 d . . . H11A H 0.4158 0.5729 0.8371 0.044 Uiso 1 1 calc R . . H11B H 0.5367 0.6191 0.8859 0.044 Uiso 1 1 calc R . . H11C H 0.4584 0.5502 0.9345 0.044 Uiso 1 1 calc R . . C12 C 0.9073(3) 0.4646(2) 0.7990(2) 0.0234(7) Uani 1 1 d . . . H12A H 0.9613 0.4146 0.8152 0.035 Uiso 1 1 calc R . . H12B H 0.9371 0.5153 0.8328 0.035 Uiso 1 1 calc R . . H12C H 0.9100 0.4773 0.7386 0.035 Uiso 1 1 calc R . . C13 C 1.0078(3) 0.2050(2) 0.6352(2) 0.0169(6) Uani 1 1 d . . . C14 C 0.9629(3) 0.1478(2) 0.5707(2) 0.0194(7) Uani 1 1 d . . . C15 C 1.0409(3) 0.1307(2) 0.5085(2) 0.0211(7) Uani 1 1 d . . . H15 H 1.0134 0.0914 0.4642 0.025 Uiso 1 1 calc R . . C16 C 1.1592(3) 0.1698(2) 0.5090(2) 0.0197(7) Uani 1 1 d . . . C17 C 1.1975(3) 0.2279(2) 0.5739(2) 0.0190(7) Uani 1 1 d . . . H17 H 1.2762 0.2563 0.5737 0.023 Uiso 1 1 calc R . . C18 C 1.1248(3) 0.2456(2) 0.6388(2) 0.0187(7) Uani 1 1 d . . . C19 C 0.8368(3) 0.1047(2) 0.5684(3) 0.0245(8) Uani 1 1 d . . . H19A H 0.8240 0.0663 0.5189 0.037 Uiso 1 1 calc R . . H19B H 0.7707 0.1491 0.5645 0.037 Uiso 1 1 calc R . . H19C H 0.8332 0.0705 0.6202 0.037 Uiso 1 1 calc R . . C20 C 1.2454(4) 0.1485(3) 0.4430(2) 0.0286(8) Uani 1 1 d . . . H20A H 1.2876 0.2016 0.4269 0.043 Uiso 1 1 calc R . . H20B H 1.1963 0.1239 0.3928 0.043 Uiso 1 1 calc R . . H20C H 1.3085 0.1062 0.4661 0.043 Uiso 1 1 calc R . . C21 C 1.1715(3) 0.3048(2) 0.7108(2) 0.0247(8) Uani 1 1 d . . . H21A H 1.1098 0.3511 0.7161 0.037 Uiso 1 1 calc R . . H21B H 1.2518 0.3306 0.6996 0.037 Uiso 1 1 calc R . . H21C H 1.1832 0.2714 0.7637 0.037 Uiso 1 1 calc R . . N1S N -0.0176(9) 0.4372(9) 0.5831(9) 0.111(6) Uani 0.50 1 d PD A -1 C1S C -0.0054(9) 0.4883(6) 0.5361(8) 0.057(3) Uani 0.50 1 d PD A -1 C2S C 0.0155(10) 0.5698(6) 0.4877(8) 0.058(4) Uani 0.50 1 d PD A -1 H2SA H 0.0063 0.5571 0.4267 0.086 Uiso 0.50 1 calc PR A -1 H2SB H 0.1004 0.5918 0.5048 0.086 Uiso 0.50 1 calc PR A -1 H2SC H -0.0464 0.6136 0.4999 0.086 Uiso 0.50 1 calc PR A -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 0.01442(14) 0.01023(14) 0.01939(15) 0.00312(10) 0.00233(10) 0.00196(10) Mo2 0.01475(14) 0.01527(15) 0.01830(15) -0.00158(10) -0.00289(10) -0.00188(10) Mo3 0.01888(15) 0.01616(15) 0.01698(15) 0.00071(10) 0.00926(11) 0.00048(11) O1 0.0140(11) 0.0109(11) 0.0179(11) 0.0008(8) 0.0019(9) -0.0020(8) O2 0.0189(12) 0.0150(12) 0.0231(12) 0.0044(9) 0.0017(9) 0.0013(9) O3 0.0156(11) 0.0133(11) 0.0159(11) 0.0039(8) 0.0036(9) 0.0004(9) O4 0.0208(12) 0.0160(11) 0.0132(11) -0.0013(8) 0.0003(9) 0.0002(9) O5 0.0182(12) 0.0226(13) 0.0270(13) -0.0042(10) -0.0049(10) -0.0047(10) O6 0.0290(14) 0.0208(13) 0.0230(13) -0.0001(10) 0.0154(10) 0.0002(10) O7 0.0162(11) 0.0142(11) 0.0168(11) 0.0029(9) -0.0033(9) 0.0001(9) O8 0.0165(11) 0.0130(11) 0.0184(11) -0.0003(9) 0.0043(9) 0.0023(9) O9 0.0097(10) 0.0159(11) 0.0221(12) 0.0008(9) 0.0045(9) -0.0003(8) O10 0.0149(15) 0.0093(14) 0.0113(14) 0.0008(11) 0.0011(11) -0.0004(11) N1 0.0129(13) 0.0145(13) 0.0203(14) 0.0022(10) 0.0048(10) 0.0003(10) N2 0.0149(13) 0.0141(14) 0.0233(14) 0.0024(11) 0.0066(11) 0.0027(10) C1 0.0169(15) 0.0126(15) 0.0161(15) 0.0004(12) -0.0009(12) 0.0002(12) C2 0.036(2) 0.025(2) 0.029(2) 0.0132(15) 0.0182(17) 0.0116(16) C3 0.032(2) 0.0234(19) 0.039(2) 0.0162(16) 0.0199(17) 0.0156(16) C4 0.0238(17) 0.0134(15) 0.0121(15) 0.0025(11) 0.0039(12) 0.0070(12) C5 0.0240(17) 0.0173(16) 0.0109(15) 0.0035(12) 0.0051(12) 0.0027(13) C6 0.0182(16) 0.0257(18) 0.0161(16) 0.0041(13) 0.0075(13) 0.0054(13) C7 0.0301(19) 0.0218(18) 0.0139(16) 0.0005(13) 0.0042(13) 0.0093(14) C8 0.0259(18) 0.0157(16) 0.0183(16) -0.0023(12) 0.0004(13) 0.0023(13) C9 0.0180(16) 0.0188(17) 0.0158(15) 0.0004(12) 0.0019(12) 0.0021(13) C10 0.0197(17) 0.0195(18) 0.0268(18) 0.0052(14) 0.0073(14) -0.0006(13) C11 0.036(2) 0.026(2) 0.0275(19) -0.0019(15) 0.0071(16) 0.0152(16) C12 0.0215(18) 0.0204(18) 0.0279(19) -0.0030(14) 0.0006(14) -0.0050(14) C13 0.0178(16) 0.0141(16) 0.0198(16) 0.0019(12) 0.0072(12) 0.0044(12) C14 0.0178(16) 0.0141(16) 0.0266(18) 0.0019(13) 0.0028(13) 0.0012(12) C15 0.0211(17) 0.0214(18) 0.0209(17) -0.0003(13) 0.0030(13) 0.0019(13) C16 0.0187(16) 0.0223(17) 0.0197(16) 0.0037(13) 0.0093(13) 0.0040(13) C17 0.0166(16) 0.0164(16) 0.0252(17) 0.0054(13) 0.0076(13) -0.0001(13) C18 0.0229(17) 0.0125(16) 0.0210(17) 0.0030(12) 0.0032(13) 0.0038(13) C19 0.0186(17) 0.0200(18) 0.036(2) -0.0055(15) 0.0060(15) 0.0003(14) C20 0.029(2) 0.036(2) 0.0236(19) -0.0031(15) 0.0131(15) -0.0014(16) C21 0.0210(17) 0.0237(19) 0.0302(19) -0.0069(15) 0.0061(14) -0.0033(14) N1S 0.042(6) 0.128(11) 0.172(14) 0.126(11) 0.056(7) 0.044(6) C1S 0.009(4) 0.096(10) 0.067(8) 0.031(7) 0.016(4) 0.012(6) C2S 0.019(5) 0.080(9) 0.076(9) 0.036(8) 0.010(5) 0.004(6) _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 O2 1.688(2) . ? Mo1 O3 1.879(2) . ? Mo1 O1 1.913(2) . ? Mo1 O7 1.948(2) . ? Mo1 O8 1.981(2) . ? Mo1 O10 2.3084(3) . ? Mo2 O5 1.685(2) . ? Mo2 O9 1.894(2) . ? Mo2 O7 1.919(2) . ? Mo2 O1 1.938(2) 3_666 ? Mo2 O4 1.957(2) . ? Mo2 O10 2.3249(3) . ? Mo3 O6 1.684(2) . ? Mo3 O4 1.889(2) 3_666 ? Mo3 O8 1.889(2) . ? Mo3 O9 1.954(2) . ? Mo3 O3 1.966(2) 3_666 ? Mo3 O10 2.3242(3) . ? O1 Mo2 1.938(2) 3_666 ? O3 Mo3 1.965(2) 3_666 ? O4 Mo3 1.889(2) 3_666 ? O10 Mo1 2.3084(3) 3_666 ? O10 Mo3 2.3242(3) 3_666 ? O10 Mo2 2.3249(3) 3_666 ? N1 C1 1.331(4) . ? N1 C2 1.381(4) . ? N1 C4 1.454(4) . ? N2 C1 1.321(4) . ? N2 C3 1.384(4) . ? N2 C13 1.449(4) . ? C2 C3 1.354(5) . ? C4 C5 1.387(5) . ? C4 C9 1.395(5) . ? C5 C6 1.390(5) . ? C5 C10 1.509(5) . ? C6 C7 1.383(5) . ? C7 C8 1.390(5) . ? C7 C11 1.501(5) . ? C8 C9 1.401(5) . ? C9 C12 1.514(5) . ? C13 C18 1.394(5) . ? C13 C14 1.395(5) . ? C14 C15 1.385(5) . ? C14 C19 1.501(5) . ? C15 C16 1.401(5) . ? C16 C17 1.391(5) . ? C16 C20 1.504(5) . ? C17 C18 1.382(5) . ? C18 C21 1.504(5) . ? N1S C1S 1.0999(10) . ? C1S C2S 1.5000(10) . ? 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 O2 Mo1 O3 103.70(11) . . ? O2 Mo1 O1 104.02(11) . . ? O3 Mo1 O1 89.38(10) . . ? O2 Mo1 O7 101.82(10) . . ? O3 Mo1 O7 88.67(10) . . ? O1 Mo1 O7 153.80(9) . . ? O2 Mo1 O8 102.22(10) . . ? O3 Mo1 O8 154.02(9) . . ? O1 Mo1 O8 86.10(9) . . ? O7 Mo1 O8 84.31(9) . . ? O2 Mo1 O10 178.00(8) . . ? O3 Mo1 O10 77.72(7) . . ? O1 Mo1 O10 77.33(7) . . ? O7 Mo1 O10 76.73(6) . . ? O8 Mo1 O10 76.32(6) . . ? O5 Mo2 O9 104.14(11) . . ? O5 Mo2 O7 103.82(11) . . ? O9 Mo2 O7 88.31(10) . . ? O5 Mo2 O1 102.80(11) . 3_666 ? O9 Mo2 O1 87.50(9) . 3_666 ? O7 Mo2 O1 153.27(9) . 3_666 ? O5 Mo2 O4 103.44(11) . . ? O9 Mo2 O4 152.39(10) . . ? O7 Mo2 O4 86.36(10) . . ? O1 Mo2 O4 85.24(9) 3_666 . ? O5 Mo2 O10 178.89(9) . . ? O9 Mo2 O10 76.70(7) . . ? O7 Mo2 O10 76.87(7) . . ? O1 Mo2 O10 76.47(6) 3_666 . ? O4 Mo2 O10 75.70(7) . . ? O6 Mo3 O4 104.07(12) . 3_666 ? O6 Mo3 O8 103.10(11) . . ? O4 Mo3 O8 90.12(10) 3_666 . ? O6 Mo3 O9 103.29(11) . . ? O4 Mo3 O9 152.40(9) 3_666 . ? O8 Mo3 O9 87.16(10) . . ? O6 Mo3 O3 103.47(11) . 3_666 ? O4 Mo3 O3 86.57(10) 3_666 3_666 ? O8 Mo3 O3 153.23(9) . 3_666 ? O9 Mo3 O3 83.67(9) . 3_666 ? O6 Mo3 O10 178.71(9) . . ? O4 Mo3 O10 76.95(7) 3_666 . ? O8 Mo3 O10 77.63(7) . . ? O9 Mo3 O10 75.64(6) . . ? O3 Mo3 O10 75.74(6) 3_666 . ? Mo1 O1 Mo2 116.23(11) . 3_666 ? Mo1 O3 Mo3 116.64(11) . 3_666 ? Mo3 O4 Mo2 117.38(11) 3_666 . ? Mo2 O7 Mo1 116.16(11) . . ? Mo3 O8 Mo1 115.84(11) . . ? Mo2 O9 Mo3 117.49(11) . . ? Mo1 O10 Mo1 180.0 . 3_666 ? Mo1 O10 Mo3 89.880(10) . 3_666 ? Mo1 O10 Mo3 90.121(10) 3_666 3_666 ? Mo1 O10 Mo3 90.119(10) . . ? Mo1 O10 Mo3 89.880(10) 3_666 . ? Mo3 O10 Mo3 180.0 3_666 . ? Mo1 O10 Mo2 89.786(10) . 3_666 ? Mo1 O10 Mo2 90.214(10) 3_666 3_666 ? Mo3 O10 Mo2 90.068(11) 3_666 3_666 ? Mo3 O10 Mo2 89.931(11) . 3_666 ? Mo1 O10 Mo2 90.215(10) . . ? Mo1 O10 Mo2 89.786(10) 3_666 . ? Mo3 O10 Mo2 89.933(11) 3_666 . ? Mo3 O10 Mo2 90.068(11) . . ? Mo2 O10 Mo2 180.0 3_666 . ? C1 N1 C2 108.4(3) . . ? C1 N1 C4 125.4(3) . . ? C2 N1 C4 126.0(3) . . ? C1 N2 C3 108.6(3) . . ? C1 N2 C13 125.0(3) . . ? C3 N2 C13 126.3(3) . . ? N2 C1 N1 109.1(3) . . ? C3 C2 N1 107.1(3) . . ? C2 C3 N2 106.8(3) . . ? C5 C4 C9 123.8(3) . . ? C5 C4 N1 118.9(3) . . ? C9 C4 N1 117.3(3) . . ? C4 C5 C6 116.8(3) . . ? C4 C5 C10 122.6(3) . . ? C6 C5 C10 120.6(3) . . ? C7 C6 C5 122.6(3) . . ? C6 C7 C8 118.2(3) . . ? C6 C7 C11 121.3(3) . . ? C8 C7 C11 120.5(3) . . ? C7 C8 C9 122.2(3) . . ? C4 C9 C8 116.3(3) . . ? C4 C9 C12 122.9(3) . . ? C8 C9 C12 120.8(3) . . ? C18 C13 C14 123.3(3) . . ? C18 C13 N2 118.1(3) . . ? C14 C13 N2 118.6(3) . . ? C15 C14 C13 117.1(3) . . ? C15 C14 C19 120.6(3) . . ? C13 C14 C19 122.3(3) . . ? C14 C15 C16 121.9(3) . . ? C17 C16 C15 118.2(3) . . ? C17 C16 C20 120.1(3) . . ? C15 C16 C20 121.6(3) . . ? C18 C17 C16 122.2(3) . . ? C17 C18 C13 117.2(3) . . ? C17 C18 C21 121.1(3) . . ? C13 C18 C21 121.7(3) . . ? N1S C1S C2S 168.2(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.810 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.125 # Attachment 'A104.cif' data_a104 _database_code_depnum_ccdc_archive 'CCDC 824845' #TrackingRef 'A104.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H24 B F4 Mo N3 O2' _chemical_formula_weight 593.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8246(12) _cell_length_b 11.9309(15) _cell_length_c 22.990(3) _cell_angle_alpha 77.187(2) _cell_angle_beta 83.435(2) _cell_angle_gamma 76.056(2) _cell_volume 2545.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 992 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 27.48 _exptl_crystal_description BLOCK _exptl_crystal_colour DARK_RED _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.574 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7394 _exptl_absorpt_correction_T_max 0.8939 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _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 '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 32965 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.91 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11682 _reflns_number_gt 10355 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+1.5460P] 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 11682 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.695090(15) 0.413408(13) 0.852575(6) 0.01401(5) Uani 1 1 d . . . Mo2 Mo 0.697506(15) 0.425068(12) 0.348545(6) 0.01283(5) Uani 1 1 d . . . O1 O 0.83057(17) 0.47955(14) 0.72475(6) 0.0298(3) Uani 1 1 d . . . O2 O 0.62648(17) 0.22855(13) 0.78885(7) 0.0305(3) Uani 1 1 d . . . O3 O 0.65255(18) 0.23596(13) 0.28161(7) 0.0331(4) Uani 1 1 d . . . O4 O 0.80904(16) 0.51648(13) 0.21938(6) 0.0250(3) Uani 1 1 d . . . N1 N 0.95461(16) 0.18786(13) 0.87851(7) 0.0162(3) Uani 1 1 d . . . N2 N 0.77804(16) 0.14868(14) 0.93585(7) 0.0171(3) Uani 1 1 d . . . N3 N 0.86816(17) 0.46368(14) 0.88397(7) 0.0186(3) Uani 1 1 d . . . N4 N 0.81152(16) 0.15704(13) 0.42251(7) 0.0159(3) Uani 1 1 d . . . N5 N 0.97993(16) 0.21823(13) 0.36745(7) 0.0152(3) Uani 1 1 d . . . N6 N 0.86397(16) 0.48401(13) 0.37925(7) 0.0171(3) Uani 1 1 d . . . C1 C 0.4779(2) 0.52643(18) 0.83018(9) 0.0237(4) Uani 1 1 d . . . H1 H 0.4343 0.5384 0.7924 0.028 Uiso 1 1 calc R . . C2 C 0.5530(2) 0.60254(18) 0.84523(10) 0.0266(4) Uani 1 1 d . . . H2 H 0.5729 0.6746 0.8193 0.032 Uiso 1 1 calc R . . C3 C 0.5778(2) 0.56411(19) 0.90656(10) 0.0258(4) Uani 1 1 d . . . H3 H 0.6239 0.6026 0.9296 0.031 Uiso 1 1 calc R . . C4 C 0.5210(2) 0.46489(18) 0.92975(9) 0.0237(4) Uani 1 1 d . . . H4 H 0.5190 0.4233 0.9716 0.028 Uiso 1 1 calc R . . C5 C 0.4590(2) 0.43992(18) 0.88250(9) 0.0230(4) Uani 1 1 d . . . H5 H 0.4017 0.3815 0.8865 0.028 Uiso 1 1 calc R . . C6 C 0.81901(19) 0.23681(16) 0.89400(8) 0.0152(3) Uani 1 1 d . . . C7 C 0.9956(2) 0.07337(17) 0.90993(8) 0.0202(4) Uani 1 1 d . . . H7 H 1.0836 0.0232 0.9069 0.024 Uiso 1 1 calc R . . C8 C 0.8849(2) 0.04851(17) 0.94546(9) 0.0202(4) Uani 1 1 d . . . H8 H 0.8805 -0.0224 0.9716 0.024 Uiso 1 1 calc R . . C9 C 1.05025(19) 0.24041(17) 0.83318(8) 0.0183(4) Uani 1 1 d . . . H9A H 1.1402 0.2281 0.8500 0.022 Uiso 1 1 calc R . . H9B H 1.0126 0.3248 0.8226 0.022 Uiso 1 1 calc R . . C10 C 1.0732(2) 0.18966(16) 0.77687(8) 0.0189(4) Uani 1 1 d . . . C11 C 1.1750(2) 0.22335(18) 0.73359(9) 0.0266(4) Uani 1 1 d . . . H11 H 1.2271 0.2744 0.7402 0.032 Uiso 1 1 calc R . . C12 C 1.1996(3) 0.1816(2) 0.68079(10) 0.0325(5) Uani 1 1 d . . . H12 H 1.2669 0.2057 0.6520 0.039 Uiso 1 1 calc R . . C13 C 1.1243(3) 0.1042(2) 0.67098(10) 0.0331(5) Uani 1 1 d . . . H13 H 1.1411 0.0758 0.6357 0.040 Uiso 1 1 calc R . . C14 C 1.0241(2) 0.0692(2) 0.71361(10) 0.0302(5) Uani 1 1 d . . . H14 H 0.9742 0.0163 0.7073 0.036 Uiso 1 1 calc R . . C15 C 0.9975(2) 0.11281(18) 0.76607(9) 0.0237(4) Uani 1 1 d . . . H15 H 0.9282 0.0902 0.7942 0.028 Uiso 1 1 calc R . . C16 C 0.64259(19) 0.15420(17) 0.97091(8) 0.0204(4) Uani 1 1 d . . . H16A H 0.5993 0.0933 0.9646 0.024 Uiso 1 1 calc R . . H16B H 0.5801 0.2300 0.9576 0.024 Uiso 1 1 calc R . . C17 C 0.66331(19) 0.13734(17) 1.03686(8) 0.0185(4) Uani 1 1 d . . . C18 C 0.7256(2) 0.21253(18) 1.05796(10) 0.0250(4) Uani 1 1 d . . . H18 H 0.7544 0.2748 1.0314 0.030 Uiso 1 1 calc R . . C19 C 0.7450(2) 0.19495(19) 1.11846(10) 0.0286(5) Uani 1 1 d . . . H19 H 0.7859 0.2459 1.1323 0.034 Uiso 1 1 calc R . . C20 C 0.7036(2) 0.1014(2) 1.15858(9) 0.0276(5) Uani 1 1 d . . . H20 H 0.7169 0.0896 1.1991 0.033 Uiso 1 1 calc R . . C21 C 0.6425(2) 0.02632(19) 1.13766(9) 0.0237(4) Uani 1 1 d . . . H21 H 0.6148 -0.0365 1.1642 0.028 Uiso 1 1 calc R . . C22 C 0.62214(19) 0.04407(17) 1.07722(9) 0.0197(4) Uani 1 1 d . . . H22 H 0.5807 -0.0068 1.0636 0.024 Uiso 1 1 calc R . . C23 C 0.7862(2) 0.45192(17) 0.77352(9) 0.0207(4) Uani 1 1 d . . . C24 C 0.6511(2) 0.29581(17) 0.81243(8) 0.0196(4) Uani 1 1 d . . . C25 C 0.9536(2) 0.49812(17) 0.89920(9) 0.0214(4) Uani 1 1 d . . . C26 C 1.0626(2) 0.54373(19) 0.91790(10) 0.0263(4) Uani 1 1 d . . . H26A H 1.1235 0.5665 0.8838 0.040 Uiso 1 1 calc R . . H26B H 1.1162 0.4838 0.9469 0.040 Uiso 1 1 calc R . . H26C H 1.0200 0.6111 0.9353 0.040 Uiso 1 1 calc R . . C27 C 0.5315(2) 0.45109(18) 0.43191(9) 0.0226(4) Uani 1 1 d . . . H27 H 0.5388 0.4035 0.4725 0.027 Uiso 1 1 calc R . . C28 C 0.5736(2) 0.55882(18) 0.41088(9) 0.0227(4) Uani 1 1 d . . . H28 H 0.6175 0.5978 0.4345 0.027 Uiso 1 1 calc R . . C29 C 0.5375(2) 0.60370(17) 0.35130(9) 0.0228(4) Uani 1 1 d . . . H29 H 0.5465 0.6809 0.3275 0.027 Uiso 1 1 calc R . . C30 C 0.4702(2) 0.52447(18) 0.33470(9) 0.0222(4) Uani 1 1 d . . . H30 H 0.4216 0.5386 0.2979 0.027 Uiso 1 1 calc R . . C31 C 0.4671(2) 0.42893(18) 0.38439(9) 0.0216(4) Uani 1 1 d . . . H31 H 0.4176 0.3655 0.3872 0.026 Uiso 1 1 calc R . . C32 C 0.84137(19) 0.25315(15) 0.38336(8) 0.0140(3) Uani 1 1 d . . . C33 C 0.9292(2) 0.06615(16) 0.43138(8) 0.0180(4) Uani 1 1 d . . . H33 H 0.9340 -0.0075 0.4563 0.022 Uiso 1 1 calc R . . C34 C 1.0352(2) 0.10456(16) 0.39718(8) 0.0178(4) Uani 1 1 d . . . H34 H 1.1279 0.0630 0.3940 0.021 Uiso 1 1 calc R . . C35 C 0.67579(19) 0.14779(17) 0.45436(8) 0.0191(4) Uani 1 1 d . . . H35A H 0.6517 0.0766 0.4492 0.023 Uiso 1 1 calc R . . H35B H 0.6041 0.2144 0.4371 0.023 Uiso 1 1 calc R . . C36 C 0.67645(19) 0.14497(16) 0.52055(8) 0.0173(4) Uani 1 1 d . . . C37 C 0.5805(2) 0.09157(19) 0.55945(9) 0.0255(4) Uani 1 1 d . . . H37 H 0.5177 0.0595 0.5445 0.031 Uiso 1 1 calc R . . C38 C 0.5784(2) 0.0861(2) 0.62043(10) 0.0305(5) Uani 1 1 d . . . H38 H 0.5135 0.0509 0.6461 0.037 Uiso 1 1 calc R . . C39 C 0.6714(2) 0.13206(18) 0.64320(9) 0.0277(5) Uani 1 1 d . . . H39 H 0.6705 0.1268 0.6842 0.033 Uiso 1 1 calc R . . C40 C 0.7664(2) 0.18620(17) 0.60487(9) 0.0258(4) Uani 1 1 d . . . H40 H 0.8288 0.2181 0.6201 0.031 Uiso 1 1 calc R . . C41 C 0.7690(2) 0.19309(16) 0.54336(9) 0.0209(4) Uani 1 1 d . . . H41 H 0.8327 0.2299 0.5177 0.025 Uiso 1 1 calc R . . C42 C 1.06796(19) 0.28761(16) 0.32543(8) 0.0178(4) Uani 1 1 d . . . H42A H 1.1393 0.3016 0.3471 0.021 Uiso 1 1 calc R . . H42B H 1.0100 0.3635 0.3086 0.021 Uiso 1 1 calc R . . C43 C 1.1384(2) 0.22708(16) 0.27543(8) 0.0197(4) Uani 1 1 d . . . C44 C 1.0636(2) 0.2268(2) 0.22735(10) 0.0310(5) Uani 1 1 d . . . H44 H 0.9687 0.2633 0.2264 0.037 Uiso 1 1 calc R . . C45 C 1.1298(3) 0.1726(2) 0.18099(10) 0.0362(5) Uani 1 1 d . . . H45 H 1.0792 0.1733 0.1490 0.043 Uiso 1 1 calc R . . C46 C 1.2705(3) 0.1176(2) 0.18211(10) 0.0340(5) Uani 1 1 d . . . H46 H 1.3148 0.0811 0.1511 0.041 Uiso 1 1 calc R . . C47 C 1.3452(2) 0.1171(2) 0.22971(11) 0.0339(5) Uani 1 1 d . . . H47 H 1.4398 0.0797 0.2308 0.041 Uiso 1 1 calc R . . C48 C 1.2792(2) 0.17230(18) 0.27598(9) 0.0267(4) Uani 1 1 d . . . H48 H 1.3304 0.1723 0.3076 0.032 Uiso 1 1 calc R . . C49 C 0.6671(2) 0.30530(17) 0.30614(9) 0.0204(4) Uani 1 1 d . . . C50 C 0.7732(2) 0.48033(16) 0.26826(8) 0.0184(4) Uani 1 1 d . . . C51 C 0.9482(2) 0.51767(17) 0.39532(9) 0.0211(4) Uani 1 1 d . . . C52 C 1.0580(2) 0.5611(2) 0.41528(10) 0.0283(5) Uani 1 1 d . . . H52A H 1.1193 0.4968 0.4393 0.042 Uiso 1 1 calc R . . H52B H 1.0158 0.6196 0.4386 0.042 Uiso 1 1 calc R . . H52C H 1.1110 0.5954 0.3811 0.042 Uiso 1 1 calc R . . B1 B 0.7764(2) 0.7591(2) 0.51288(10) 0.0223(4) Uani 1 1 d . . . F1 F 0.26864(18) 0.24897(14) 0.93134(6) 0.0449(4) Uani 1 1 d . . . F2 F 0.26350(17) 0.33806(12) 1.00923(7) 0.0405(3) Uani 1 1 d . . . F3 F 0.09197(14) 0.24420(13) 1.00386(8) 0.0464(4) Uani 1 1 d . . . F4 F 0.31247(14) 0.13772(11) 1.02334(6) 0.0337(3) Uani 1 1 d . . . B2 B 0.2343(3) 0.2410(2) 0.99214(11) 0.0250(5) Uani 1 1 d . . . F5 F 0.73235(16) 0.67412(12) 0.49119(6) 0.0378(3) Uani 1 1 d . . . F6 F 0.91903(14) 0.71839(12) 0.52280(6) 0.0373(3) Uani 1 1 d . . . F7 F 0.70139(15) 0.77615(13) 0.56605(6) 0.0366(3) Uani 1 1 d . . . F8 F 0.75660(15) 0.86394(11) 0.47142(6) 0.0376(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01621(9) 0.01396(8) 0.01194(8) -0.00263(6) -0.00230(6) -0.00283(6) Mo2 0.01462(8) 0.01284(8) 0.01101(8) -0.00320(6) -0.00099(6) -0.00222(6) O1 0.0384(9) 0.0353(8) 0.0178(7) -0.0008(6) 0.0012(6) -0.0177(7) O2 0.0375(9) 0.0273(8) 0.0317(8) -0.0128(7) -0.0099(7) -0.0069(7) O3 0.0469(10) 0.0243(8) 0.0329(9) -0.0135(7) -0.0148(7) -0.0044(7) O4 0.0319(8) 0.0270(7) 0.0149(7) -0.0014(6) 0.0009(6) -0.0081(6) N1 0.0157(7) 0.0178(7) 0.0147(7) -0.0041(6) -0.0014(6) -0.0021(6) N2 0.0164(8) 0.0186(7) 0.0149(7) -0.0001(6) -0.0024(6) -0.0035(6) N3 0.0209(8) 0.0176(7) 0.0178(8) -0.0047(6) 0.0005(6) -0.0049(6) N4 0.0183(8) 0.0155(7) 0.0141(7) -0.0025(6) -0.0025(6) -0.0040(6) N5 0.0170(7) 0.0152(7) 0.0127(7) -0.0029(6) -0.0017(6) -0.0020(6) N6 0.0196(8) 0.0160(7) 0.0162(7) -0.0050(6) 0.0010(6) -0.0043(6) C1 0.0227(10) 0.0247(10) 0.0208(10) -0.0049(8) -0.0075(8) 0.0033(8) C2 0.0281(11) 0.0160(9) 0.0318(11) -0.0042(8) -0.0026(9) 0.0020(8) C3 0.0223(10) 0.0269(10) 0.0303(11) -0.0170(9) -0.0034(8) 0.0011(8) C4 0.0234(10) 0.0283(10) 0.0174(9) -0.0086(8) 0.0009(8) 0.0008(8) C5 0.0182(9) 0.0236(10) 0.0276(10) -0.0084(8) -0.0004(8) -0.0026(8) C6 0.0172(9) 0.0179(8) 0.0115(8) -0.0030(7) -0.0027(6) -0.0052(7) C7 0.0207(9) 0.0187(9) 0.0186(9) -0.0025(7) -0.0048(7) 0.0011(7) C8 0.0219(10) 0.0174(9) 0.0194(9) -0.0010(7) -0.0053(7) -0.0011(7) C9 0.0171(9) 0.0216(9) 0.0167(9) -0.0048(7) 0.0009(7) -0.0054(7) C10 0.0212(9) 0.0173(9) 0.0165(9) -0.0042(7) 0.0008(7) -0.0016(7) C11 0.0296(11) 0.0254(10) 0.0273(11) -0.0100(8) 0.0056(9) -0.0103(8) C12 0.0416(13) 0.0315(11) 0.0246(11) -0.0088(9) 0.0102(9) -0.0111(10) C13 0.0449(14) 0.0338(12) 0.0223(11) -0.0121(9) -0.0019(9) -0.0065(10) C14 0.0373(12) 0.0314(11) 0.0264(11) -0.0102(9) -0.0053(9) -0.0106(9) C15 0.0232(10) 0.0292(10) 0.0193(9) -0.0058(8) -0.0014(8) -0.0061(8) C16 0.0147(9) 0.0236(9) 0.0209(9) 0.0014(7) -0.0028(7) -0.0050(7) C17 0.0134(8) 0.0205(9) 0.0200(9) -0.0045(7) 0.0007(7) -0.0009(7) C18 0.0243(10) 0.0199(9) 0.0310(11) -0.0043(8) -0.0051(8) -0.0042(8) C19 0.0274(11) 0.0263(10) 0.0348(12) -0.0148(9) -0.0067(9) -0.0012(8) C20 0.0226(10) 0.0390(12) 0.0199(10) -0.0137(9) 0.0008(8) 0.0015(9) C21 0.0173(9) 0.0310(11) 0.0192(9) -0.0044(8) 0.0051(7) -0.0016(8) C22 0.0152(9) 0.0239(9) 0.0204(9) -0.0059(7) 0.0015(7) -0.0048(7) C23 0.0259(10) 0.0188(9) 0.0193(9) -0.0026(7) -0.0051(8) -0.0081(8) C24 0.0211(9) 0.0194(9) 0.0170(9) -0.0013(7) -0.0052(7) -0.0021(7) C25 0.0240(10) 0.0191(9) 0.0211(9) -0.0064(7) 0.0013(8) -0.0042(8) C26 0.0238(10) 0.0286(11) 0.0301(11) -0.0100(9) -0.0016(8) -0.0087(8) C27 0.0209(10) 0.0289(10) 0.0169(9) -0.0083(8) 0.0047(7) -0.0025(8) C28 0.0184(9) 0.0274(10) 0.0258(10) -0.0172(8) 0.0035(8) -0.0031(8) C29 0.0219(10) 0.0172(9) 0.0261(10) -0.0055(8) 0.0021(8) 0.0014(7) C30 0.0165(9) 0.0259(10) 0.0223(10) -0.0070(8) -0.0022(7) 0.0009(7) C31 0.0170(9) 0.0232(9) 0.0259(10) -0.0097(8) 0.0028(8) -0.0048(7) C32 0.0180(9) 0.0142(8) 0.0104(8) -0.0029(6) -0.0022(6) -0.0035(7) C33 0.0216(9) 0.0159(8) 0.0150(8) -0.0017(7) -0.0045(7) -0.0009(7) C34 0.0201(9) 0.0150(8) 0.0170(9) -0.0044(7) -0.0033(7) 0.0006(7) C35 0.0172(9) 0.0213(9) 0.0189(9) -0.0013(7) -0.0002(7) -0.0076(7) C36 0.0188(9) 0.0143(8) 0.0168(9) -0.0023(7) 0.0010(7) -0.0015(7) C37 0.0221(10) 0.0298(11) 0.0247(10) -0.0024(8) 0.0009(8) -0.0096(8) C38 0.0280(11) 0.0352(12) 0.0225(10) -0.0016(9) 0.0086(8) -0.0048(9) C39 0.0353(12) 0.0236(10) 0.0173(10) -0.0046(8) 0.0008(8) 0.0059(9) C40 0.0353(12) 0.0181(9) 0.0240(10) -0.0058(8) -0.0049(9) -0.0032(8) C41 0.0246(10) 0.0166(9) 0.0208(9) -0.0024(7) -0.0011(8) -0.0049(7) C42 0.0174(9) 0.0175(9) 0.0182(9) -0.0039(7) 0.0007(7) -0.0040(7) C43 0.0229(10) 0.0164(8) 0.0177(9) -0.0021(7) 0.0040(7) -0.0041(7) C44 0.0305(12) 0.0351(12) 0.0256(11) -0.0111(9) -0.0022(9) 0.0011(9) C45 0.0459(14) 0.0383(13) 0.0240(11) -0.0122(10) -0.0021(10) -0.0030(11) C46 0.0460(14) 0.0280(11) 0.0253(11) -0.0101(9) 0.0168(10) -0.0073(10) C47 0.0269(11) 0.0329(12) 0.0354(12) -0.0077(10) 0.0115(9) 0.0000(9) C48 0.0242(10) 0.0286(10) 0.0253(10) -0.0055(8) 0.0029(8) -0.0042(8) C49 0.0232(10) 0.0188(9) 0.0179(9) -0.0010(7) -0.0067(7) -0.0020(7) C50 0.0218(9) 0.0156(8) 0.0188(9) -0.0053(7) -0.0026(7) -0.0036(7) C51 0.0233(10) 0.0192(9) 0.0205(9) -0.0070(7) 0.0005(8) -0.0023(8) C52 0.0257(11) 0.0306(11) 0.0341(12) -0.0147(9) -0.0024(9) -0.0088(9) B1 0.0255(11) 0.0224(11) 0.0218(11) -0.0062(9) -0.0028(9) -0.0081(9) F1 0.0722(11) 0.0468(9) 0.0253(7) -0.0067(6) -0.0057(7) -0.0308(8) F2 0.0622(10) 0.0286(7) 0.0400(8) -0.0083(6) -0.0213(7) -0.0184(7) F3 0.0263(7) 0.0368(8) 0.0787(12) -0.0203(8) -0.0038(7) -0.0038(6) F4 0.0343(7) 0.0281(7) 0.0373(7) -0.0041(6) -0.0089(6) -0.0037(5) B2 0.0290(12) 0.0224(11) 0.0263(12) -0.0050(9) -0.0078(9) -0.0078(9) F5 0.0489(9) 0.0333(7) 0.0410(8) -0.0124(6) -0.0145(7) -0.0178(6) F6 0.0287(7) 0.0405(8) 0.0465(8) -0.0205(7) -0.0114(6) -0.0001(6) F7 0.0413(8) 0.0438(8) 0.0295(7) -0.0116(6) 0.0094(6) -0.0201(6) F8 0.0471(8) 0.0283(7) 0.0343(7) 0.0052(6) -0.0037(6) -0.0128(6) _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 C23 1.942(2) . ? Mo1 C24 1.991(2) . ? Mo1 N3 2.1763(16) . ? Mo1 C6 2.2287(18) . ? Mo1 C1 2.278(2) . ? Mo1 C5 2.309(2) . ? Mo1 C2 2.332(2) . ? Mo1 C4 2.395(2) . ? Mo1 C3 2.401(2) . ? Mo2 C50 1.9436(19) . ? Mo2 C49 1.993(2) . ? Mo2 N6 2.1693(16) . ? Mo2 C32 2.2313(17) . ? Mo2 C30 2.2837(19) . ? Mo2 C31 2.3121(19) . ? Mo2 C29 2.3322(19) . ? Mo2 C27 2.3945(19) . ? Mo2 C28 2.4002(19) . ? O1 C23 1.162(2) . ? O2 C24 1.146(2) . ? O3 C49 1.143(2) . ? O4 C50 1.158(2) . ? N1 C6 1.361(2) . ? N1 C7 1.383(2) . ? N1 C9 1.460(2) . ? N2 C6 1.364(2) . ? N2 C8 1.382(2) . ? N2 C16 1.470(2) . ? N3 C25 1.137(3) . ? N4 C32 1.362(2) . ? N4 C33 1.381(2) . ? N4 C35 1.462(2) . ? N5 C32 1.357(2) . ? N5 C34 1.386(2) . ? N5 C42 1.472(2) . ? N6 C51 1.131(3) . ? C1 C2 1.417(3) . ? C1 C5 1.427(3) . ? C2 C3 1.413(3) . ? C3 C4 1.403(3) . ? C4 C5 1.422(3) . ? C7 C8 1.336(3) . ? C9 C10 1.519(3) . ? C10 C15 1.388(3) . ? C10 C11 1.393(3) . ? C11 C12 1.387(3) . ? C12 C13 1.383(3) . ? C13 C14 1.378(3) . ? C14 C15 1.391(3) . ? C16 C17 1.515(3) . ? C17 C22 1.391(3) . ? C17 C18 1.393(3) . ? C18 C19 1.388(3) . ? C19 C20 1.392(3) . ? C20 C21 1.383(3) . ? C21 C22 1.389(3) . ? C25 C26 1.455(3) . ? C27 C28 1.411(3) . ? C27 C31 1.425(3) . ? C28 C29 1.408(3) . ? C29 C30 1.413(3) . ? C30 C31 1.427(3) . ? C33 C34 1.340(3) . ? C35 C36 1.515(3) . ? C36 C41 1.388(3) . ? C36 C37 1.392(3) . ? C37 C38 1.387(3) . ? C38 C39 1.374(3) . ? C39 C40 1.384(3) . ? C40 C41 1.396(3) . ? C42 C43 1.506(3) . ? C43 C48 1.381(3) . ? C43 C44 1.396(3) . ? C44 C45 1.386(3) . ? C45 C46 1.381(3) . ? C46 C47 1.384(4) . ? C47 C48 1.390(3) . ? C51 C52 1.459(3) . ? B1 F8 1.381(3) . ? B1 F7 1.382(3) . ? B1 F6 1.395(3) . ? B1 F5 1.396(3) . ? F1 B2 1.387(3) . ? F2 B2 1.402(3) . ? F3 B2 1.387(3) . ? F4 B2 1.378(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 C23 Mo1 C24 78.63(8) . . ? C23 Mo1 N3 85.17(7) . . ? C24 Mo1 N3 142.59(7) . . ? C23 Mo1 C6 105.24(7) . . ? C24 Mo1 C6 72.72(7) . . ? N3 Mo1 C6 79.53(6) . . ? C23 Mo1 C1 96.56(8) . . ? C24 Mo1 C1 87.21(8) . . ? N3 Mo1 C1 128.32(7) . . ? C6 Mo1 C1 146.38(7) . . ? C23 Mo1 C5 129.88(8) . . ? C24 Mo1 C5 82.42(8) . . ? N3 Mo1 C5 132.25(7) . . ? C6 Mo1 C5 112.58(7) . . ? C1 Mo1 C5 36.25(7) . . ? C23 Mo1 C2 92.88(8) . . ? C24 Mo1 C2 121.47(8) . . ? N3 Mo1 C2 92.59(7) . . ? C6 Mo1 C2 159.40(7) . . ? C1 Mo1 C2 35.78(8) . . ? C5 Mo1 C2 59.46(7) . . ? C23 Mo1 C4 150.82(8) . . ? C24 Mo1 C4 112.58(8) . . ? N3 Mo1 C4 97.91(7) . . ? C6 Mo1 C4 103.84(7) . . ? C1 Mo1 C4 58.87(7) . . ? C5 Mo1 C4 35.13(7) . . ? C2 Mo1 C4 58.08(7) . . ? C23 Mo1 C3 121.44(8) . . ? C24 Mo1 C3 140.00(8) . . ? N3 Mo1 C3 76.89(7) . . ? C6 Mo1 C3 124.74(7) . . ? C1 Mo1 C3 58.29(7) . . ? C5 Mo1 C3 57.93(7) . . ? C2 Mo1 C3 34.70(7) . . ? C4 Mo1 C3 34.02(7) . . ? C50 Mo2 C49 78.78(8) . . ? C50 Mo2 N6 86.01(7) . . ? C49 Mo2 N6 141.37(7) . . ? C50 Mo2 C32 105.99(7) . . ? C49 Mo2 C32 71.72(7) . . ? N6 Mo2 C32 78.89(6) . . ? C50 Mo2 C30 96.76(8) . . ? C49 Mo2 C30 89.11(8) . . ? N6 Mo2 C30 128.13(7) . . ? C32 Mo2 C30 146.25(7) . . ? C50 Mo2 C31 129.80(8) . . ? C49 Mo2 C31 83.32(8) . . ? N6 Mo2 C31 131.85(6) . . ? C32 Mo2 C31 112.10(7) . . ? C30 Mo2 C31 36.17(7) . . ? C50 Mo2 C29 93.47(7) . . ? C49 Mo2 C29 123.40(8) . . ? N6 Mo2 C29 92.54(7) . . ? C32 Mo2 C29 157.96(7) . . ? C30 Mo2 C29 35.64(7) . . ? C31 Mo2 C29 59.29(7) . . ? C50 Mo2 C27 151.47(7) . . ? C49 Mo2 C27 112.74(8) . . ? N6 Mo2 C27 97.47(6) . . ? C32 Mo2 C27 102.45(7) . . ? C30 Mo2 C27 58.96(7) . . ? C31 Mo2 C27 35.20(7) . . ? C29 Mo2 C27 58.17(7) . . ? C50 Mo2 C28 121.98(7) . . ? C49 Mo2 C28 141.10(8) . . ? N6 Mo2 C28 76.57(6) . . ? C32 Mo2 C28 123.42(7) . . ? C30 Mo2 C28 58.17(7) . . ? C31 Mo2 C28 57.94(7) . . ? C29 Mo2 C28 34.58(7) . . ? C27 Mo2 C28 34.24(7) . . ? C6 N1 C7 111.49(15) . . ? C6 N1 C9 127.67(15) . . ? C7 N1 C9 120.78(15) . . ? C6 N2 C8 111.66(15) . . ? C6 N2 C16 127.31(16) . . ? C8 N2 C16 120.94(15) . . ? C25 N3 Mo1 175.09(16) . . ? C32 N4 C33 111.50(15) . . ? C32 N4 C35 126.44(15) . . ? C33 N4 C35 122.02(15) . . ? C32 N5 C34 111.37(15) . . ? C32 N5 C42 127.16(15) . . ? C34 N5 C42 121.47(15) . . ? C51 N6 Mo2 178.08(15) . . ? C2 C1 C5 108.02(18) . . ? C2 C1 Mo1 74.15(12) . . ? C5 C1 Mo1 73.05(11) . . ? C3 C2 C1 107.46(19) . . ? C3 C2 Mo1 75.34(12) . . ? C1 C2 Mo1 70.07(11) . . ? C4 C3 C2 109.16(19) . . ? C4 C3 Mo1 72.74(11) . . ? C2 C3 Mo1 69.96(11) . . ? C3 C4 C5 107.79(18) . . ? C3 C4 Mo1 73.24(12) . . ? C5 C4 Mo1 69.14(11) . . ? C4 C5 C1 107.56(18) . . ? C4 C5 Mo1 75.72(12) . . ? C1 C5 Mo1 70.71(11) . . ? N1 C6 N2 103.22(15) . . ? N1 C6 Mo1 126.50(13) . . ? N2 C6 Mo1 130.05(13) . . ? C8 C7 N1 106.97(17) . . ? C7 C8 N2 106.66(16) . . ? N1 C9 C10 113.15(15) . . ? C15 C10 C11 118.48(18) . . ? C15 C10 C9 123.63(17) . . ? C11 C10 C9 117.89(17) . . ? C12 C11 C10 120.8(2) . . ? C13 C12 C11 120.0(2) . . ? C14 C13 C12 119.9(2) . . ? C13 C14 C15 120.1(2) . . ? C10 C15 C14 120.74(19) . . ? N2 C16 C17 110.49(15) . . ? C22 C17 C18 119.02(18) . . ? C22 C17 C16 119.84(17) . . ? C18 C17 C16 121.13(18) . . ? C19 C18 C17 120.3(2) . . ? C18 C19 C20 120.4(2) . . ? C21 C20 C19 119.4(2) . . ? C20 C21 C22 120.37(19) . . ? C21 C22 C17 120.54(19) . . ? O1 C23 Mo1 174.73(18) . . ? O2 C24 Mo1 179.37(18) . . ? N3 C25 C26 179.1(2) . . ? C28 C27 C31 107.23(18) . . ? C28 C27 Mo2 73.10(11) . . ? C31 C27 Mo2 69.24(11) . . ? C29 C28 C27 109.22(18) . . ? C29 C28 Mo2 70.07(11) . . ? C27 C28 Mo2 72.66(11) . . ? C28 C29 C30 107.78(18) . . ? C28 C29 Mo2 75.35(11) . . ? C30 C29 Mo2 70.31(11) . . ? C29 C30 C31 107.97(18) . . ? C29 C30 Mo2 74.05(11) . . ? C31 C30 Mo2 73.00(11) . . ? C27 C31 C30 107.79(17) . . ? C27 C31 Mo2 75.56(11) . . ? C30 C31 Mo2 70.83(11) . . ? N5 C32 N4 103.62(15) . . ? N5 C32 Mo2 127.17(12) . . ? N4 C32 Mo2 129.13(13) . . ? C34 C33 N4 106.71(16) . . ? C33 C34 N5 106.78(16) . . ? N4 C35 C36 112.44(15) . . ? C41 C36 C37 119.37(18) . . ? C41 C36 C35 122.40(17) . . ? C37 C36 C35 118.23(17) . . ? C38 C37 C36 120.1(2) . . ? C39 C38 C37 120.6(2) . . ? C38 C39 C40 119.73(19) . . ? C39 C40 C41 120.3(2) . . ? C36 C41 C40 119.91(18) . . ? N5 C42 C43 112.62(15) . . ? C48 C43 C44 118.80(19) . . ? C48 C43 C42 120.29(18) . . ? C44 C43 C42 120.90(18) . . ? C45 C44 C43 120.6(2) . . ? C46 C45 C44 120.2(2) . . ? C45 C46 C47 119.6(2) . . ? C46 C47 C48 120.2(2) . . ? C43 C48 C47 120.6(2) . . ? O3 C49 Mo2 178.62(19) . . ? O4 C50 Mo2 175.36(17) . . ? N6 C51 C52 179.2(2) . . ? F8 B1 F7 109.88(18) . . ? F8 B1 F6 109.53(18) . . ? F7 B1 F6 109.46(18) . . ? F8 B1 F5 109.94(18) . . ? F7 B1 F5 109.81(18) . . ? F6 B1 F5 108.20(18) . . ? F4 B2 F3 110.33(19) . . ? F4 B2 F1 109.60(19) . . ? F3 B2 F1 109.63(19) . . ? F4 B2 F2 109.99(18) . . ? F3 B2 F2 108.59(19) . . ? F1 B2 F2 108.68(18) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.927 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.085