# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jeffrey Long' _publ_contact_author_email JRLONG@BERKELEY.EDU _publ_section_title ; Strong Magnetic Exchange Coupling in the Cyano-Bridged Coordination Clusters [(PY5Me2)4V4M(CN)6]5+ (M = Cr, Mo) ; loop_ _publ_author_name 'Jeffrey Long' 'Danna E Freedman' 'David M Jenkins' # Attachment '14.cif' data_df98a _database_code_depnum_ccdc_archive 'CCDC 730661' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C137 H100 Cr1 F28.5 N33.5 O1.2 P5 V4' _chemical_formula_weight 3183.6064 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4/mcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z+1/2' 'x, -y, -z+1/2' 'y, x, -z+1/2' '-y, -x, -z+1/2' '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' '-x+1/2, y+1/2, -z+1' 'x+1/2, -y+1/2, -z+1' 'y+1/2, x+1/2, -z+1' '-y+1/2, -x+1/2, -z+1' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z-1/2' '-x, y, z-1/2' '-y, -x, z-1/2' 'y, x, z-1/2' '-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' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 33.3070(10) _cell_length_b 33.3070(10) _cell_length_c 28.8894(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 32049(2) _cell_formula_units_Z 8 _cell_measurement_temperature 156 _cell_measurement_reflns_used 6533 _cell_measurement_theta_min 4.463 _cell_measurement_theta_max 52.544 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max .2 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12911 _exptl_absorpt_coefficient_mu 0.43 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.835758 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; It is extremely difficult to obtain high-quality crystals of these compounds owing to the size and charge of the polynuclear coordination clusters. Many crystals were examined in an effort to obtain the best quality data. In situations in which a central cluster is surrounded by anion and solvent disorder, frequently the parameters of goodness of fit and wR2 are less than ideal. We believe the structures reported treat the available data in an appropriate manner, and this has been confirmed by consultation with our departmental crystallographer, Dr. Fred Hollander. ; _diffrn_ambient_temperature 156 _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 SMART CCD' _diffrn_measurement_method \w/2\q-scans _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 70168 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0148 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 23.28 _reflns_number_total 6071 _reflns_number_gt 4749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v6.36' _computing_data_reduction 'Bruker SAINT v6.36' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6071 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_gt 0.0989 _refine_ls_wR_factor_ref 0.3159 _refine_ls_wR_factor_gt 0.2882 _refine_ls_goodness_of_fit_ref 2.675 _refine_ls_restrained_S_all 2.675 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.25380(4) 0.24620(4) 0.5000 0.0318(5) Uani 1 4 d S . . V1 V 0.16225(4) 0.11996(4) 0.5000 0.0254(4) Uani 1 2 d S . . V2 V 0.19322(3) 0.30678(3) 0.35183(5) 0.0368(5) Uani 1 2 d S . . P1 P 0.0000 0.0000 0.36844(12) 0.0379(8) Uani 1 4 d S . . P2 P 0.17255(8) 0.0000 0.2500 0.0410(6) Uani 1 2 d S . . P3 P 0.0912(2) 0.4088(2) 0.5000 0.153(3) Uani 1 4 d S . . P4 P 0.1446(4) 0.5303(4) 0.5188(4) 0.110(4) Uiso 0.25 1 d P . . F1 F -0.04365(13) 0.01973(12) 0.36789(14) 0.0595(11) Uiso 1 1 d . . . F2 F 0.0000 0.0000 0.3136(3) 0.066(2) Uiso 1 4 d S . . F3 F -0.005(2) -0.0084(16) 0.4233(3) 0.045(4) Uiso 0.25 1 d P . . F4 F 0.17271(11) -0.04527(12) 0.23308(13) 0.0537(10) Uiso 1 1 d . . . F5 F 0.13825(13) 0.01000(13) 0.21344(14) 0.0601(11) Uiso 1 1 d . . . F6 F 0.20530(13) 0.01024(14) 0.21211(15) 0.0672(12) Uiso 1 1 d . . . F7 F 0.0556(6) 0.4444(6) 0.5000 0.250(11) Uiso 1 4 d S . . F8 F 0.0891(4) 0.4109(4) 0.4436(8) 0.250(8) Uiso 1 2 d S . . F9 F 0.1225(4) 0.3775(4) 0.5000 0.133(5) Uiso 1 4 d S . . F10 F 0.1215(6) 0.4454(6) 0.5000 0.230(7) Uiso 1 2 d S . . F11 F 0.1733(7) 0.5621(8) 0.5000 0.065(6) Uiso 0.25 2 d SP . . F12 F 0.1516(9) 0.4888(9) 0.5000 0.088(8) Uiso 0.25 2 d SP . . F13 F 0.1064(9) 0.5431(9) 0.5000 0.086(8) Uiso 0.25 2 d SP . . F14 F 0.1852(11) 0.5145(11) 0.5386(14) 0.155(14) Uiso 0.25 1 d P . . F15 F 0.1152(18) 0.5191(19) 0.553(2) 0.26(2) Uiso 0.25 1 d P . . F16 F 0.1336(16) 0.5598(17) 0.5557(18) 0.131(15) Uiso 0.15 1 d P . . C1 C 0.2124(3) 0.2009(3) 0.5000 0.0328(19) Uani 1 2 d S . . C2 C 0.22303(19) 0.27697(19) 0.4499(3) 0.0351(19) Uani 1 2 d S . . C3 C 0.2848(2) 0.2152(2) 0.4494(3) 0.041(2) Uani 1 2 d S . . C10 C 0.12180(17) 0.04732(17) 0.45931(19) 0.0330(13) Uani 1 1 d . . . C11 C 0.18056(17) 0.07398(17) 0.41155(18) 0.0314(13) Uani 1 1 d . . . C12 C 0.11381(16) 0.11039(17) 0.41162(18) 0.0301(13) Uani 1 1 d . . . C13 C 0.26718(19) 0.34460(19) 0.3071(2) 0.0400(15) Uani 1 1 d . . . C14 C 0.23732(18) 0.1047(2) 0.4404(2) 0.0381(14) Uani 1 1 d . . . H14A H 0.2491 0.1214 0.4624 0.046 Uiso 1 1 calc R . . C15 C 0.11071(19) 0.1754(2) 0.4400(2) 0.0428(15) Uani 1 1 d . . . H15A H 0.1191 0.1942 0.4618 0.051 Uiso 1 1 calc R . . C16 C 0.26148(19) 0.0893(2) 0.4065(2) 0.0463(17) Uani 1 1 d . . . H16A H 0.2885 0.0962 0.4045 0.056 Uiso 1 1 calc R . . C17 C 0.08705(19) 0.1208(2) 0.3766(2) 0.0444(16) Uani 1 1 d . . . H17A H 0.0790 0.1018 0.3550 0.053 Uiso 1 1 calc R . . C18 C 0.1485(2) 0.3011(2) 0.2118(2) 0.0491(17) Uani 1 1 d . . . H18A H 0.1297 0.2855 0.1962 0.059 Uiso 1 1 calc R . . C19 C 0.13398(17) 0.06874(17) 0.41379(18) 0.0320(13) Uani 1 1 d . . . C20 C 0.1203(2) 0.0433(2) 0.3725(2) 0.0439(16) Uani 1 1 d . . . H20A H 0.1280 0.0563 0.3442 0.066 Uiso 1 1 calc R . . H20B H 0.0916 0.0404 0.3733 0.066 Uiso 1 1 calc R . . H20C H 0.1326 0.0173 0.3741 0.066 Uiso 1 1 calc R . . C21 C 0.1004(2) 0.0112(2) 0.4588(2) 0.0464(17) Uani 1 1 d . . . H21A H 0.0935 -0.0009 0.4309 0.056 Uiso 1 1 calc R . . C22 C 0.0850(2) 0.1878(2) 0.4061(2) 0.0518(18) Uani 1 1 d . . . H22A H 0.0763 0.2143 0.4045 0.062 Uiso 1 1 calc R . . C23 C 0.2031(2) 0.05641(19) 0.3774(2) 0.0400(15) Uani 1 1 d . . . H23A H 0.1908 0.0400 0.3555 0.048 Uiso 1 1 calc R . . C24 C 0.2333(2) 0.37194(19) 0.2872(2) 0.0432(16) Uani 1 1 d . . . C25 C 0.15299(19) 0.2970(2) 0.2593(2) 0.0421(15) Uani 1 1 d . . . C26 C 0.21305(18) 0.39324(19) 0.3279(2) 0.0416(15) Uani 1 1 d . . . C27 C 0.0899(3) -0.0062(3) 0.5000 0.049(2) Uani 1 2 d S . . H27A H 0.0754 -0.0301 0.5000 0.059 Uiso 1 2 calc SR . . C28 C 0.3070(2) 0.3531(2) 0.2986(2) 0.0496(17) Uani 1 1 d . . . H28A H 0.3144 0.3747 0.2801 0.060 Uiso 1 1 calc R . . C29 C 0.2442(2) 0.0631(2) 0.3753(2) 0.0477(17) Uani 1 1 d . . . H29A H 0.2599 0.0501 0.3533 0.057 Uiso 1 1 calc R . . C30 C 0.0725(2) 0.1598(2) 0.3741(2) 0.0512(19) Uani 1 1 d . . . H30A H 0.0544 0.1669 0.3511 0.061 Uiso 1 1 calc R . . C31 C 0.1717(2) 0.3283(2) 0.1876(3) 0.057(3) Uani 1 2 d S . . H31A H 0.1691 0.3309 0.1557 0.069 Uiso 1 2 calc SR . . C32 C 0.1958(2) 0.4525(2) 0.3711(3) 0.065(2) Uani 1 1 d . . . H32A H 0.1939 0.4803 0.3730 0.078 Uiso 1 1 calc R . . C33 C 0.2841(2) 0.2912(2) 0.3533(2) 0.0452(16) Uani 1 1 d . . . H33A H 0.2766 0.2698 0.3720 0.054 Uiso 1 1 calc R . . C34 C 0.3241(2) 0.2981(2) 0.3462(2) 0.0523(18) Uani 1 1 d . . . H34A H 0.3431 0.2818 0.3606 0.063 Uiso 1 1 calc R . . C35 C 0.3362(2) 0.3280(2) 0.3190(3) 0.0543(19) Uani 1 1 d . . . H35A H 0.3634 0.3322 0.3134 0.065 Uiso 1 1 calc R . . C36 C 0.1846(2) 0.3874(2) 0.4013(3) 0.0555(19) Uani 1 1 d . . . H36A H 0.1760 0.3711 0.4255 0.067 Uiso 1 1 calc R . . C37 C 0.2516(2) 0.4042(2) 0.2548(3) 0.0556(19) Uani 1 1 d . . . H37A H 0.2305 0.4207 0.2425 0.083 Uiso 1 1 calc R . . H37B H 0.2655 0.3913 0.2298 0.083 Uiso 1 1 calc R . . H37C H 0.2701 0.4206 0.2719 0.083 Uiso 1 1 calc R . . C38 C 0.1828(2) 0.4291(2) 0.4070(3) 0.064(2) Uani 1 1 d . . . H38A H 0.1732 0.4405 0.4342 0.077 Uiso 1 1 calc R . . C39 C 0.2115(2) 0.4351(2) 0.3325(3) 0.0528(18) Uani 1 1 d . . . H39A H 0.2214 0.4512 0.3088 0.063 Uiso 1 1 calc R . . C800 C 0.0875(2) 0.0875(2) 0.2500 0.055(3) Uiso 1 2 d S . . C801 C 0.0574(3) 0.0574(3) 0.2500 0.070(3) Uiso 1 2 d S . . C802 C 0.2540(5) 0.4643(6) 0.5000 0.112(5) Uiso 1 2 d S . . C803 C 0.2694(7) 0.5023(8) 0.5000 0.153(8) Uiso 1 2 d S . . C805 C 0.0731(17) 0.4269(17) 0.365(3) 0.25(3) Uiso 0.50 2 d SP . . C806 C 0.1505(15) 0.6286(15) 0.5000 0.082(15) Uiso 0.25 2 d SP . . N807 N 0.1255(13) 0.6255(13) 0.595(2) 0.121(19) Uiso 0.25 2 d SP . . N1 N 0.1919(2) 0.1735(2) 0.5000 0.0357(17) Uani 1 2 d S . . N2 N 0.20824(17) 0.29176(17) 0.4194(3) 0.0413(18) Uani 1 2 d S . . N3 N 0.3023(2) 0.1977(2) 0.4219(3) 0.060(2) Uani 1 2 d S . . N5 N 0.19766(13) 0.09738(13) 0.44424(15) 0.0277(11) Uani 1 1 d . . . N6 N 0.13221(19) 0.06458(19) 0.5000 0.0267(14) Uani 1 2 d S . . N7 N 0.12465(13) 0.13742(15) 0.44375(16) 0.0329(11) Uani 1 1 d . . . N8 N 0.19795(16) 0.37017(16) 0.36256(18) 0.0428(13) Uani 1 1 d . . . N9 N 0.18077(15) 0.31923(15) 0.2820(2) 0.0372(17) Uani 1 2 d S . . N10 N 0.25560(15) 0.31386(16) 0.33448(17) 0.0418(13) Uani 1 1 d . . . N800 N 0.1122(2) 0.1122(2) 0.2500 0.080(3) Uiso 1 2 d S . . N801 N 0.2494(4) 0.4302(5) 0.5000 0.105(4) Uiso 1 2 d S . . C804 C 0.0934(8) 0.4066(8) 0.3225(15) 0.212(14) Uiso 1 2 d S . . F161 F 0.1753(15) 0.5205(14) 0.5565(17) 0.007(10) Uiso 0.05 1 d P . . F162 F 0.151(3) 0.533(2) 0.568(3) 0.052(18) Uiso 0.05 1 d P . . O800 O 0.0000 0.5000 0.2500 0.092(12) Uiso 0.48 8 d SP . . C810 C 0.0315(9) 0.4685(9) 0.2463(13) 0.051(10) Uiso 0.25 2 d SP . . N802 N 0.1068(7) 0.3932(7) 0.2931(12) 0.235(13) Uiso 1 2 d S . . C807 C 0.1355(9) 0.6355(9) 0.5618(16) 0.130(13) Uiso 0.50 2 d SP . . O810 O 0.0000 0.5000 0.2845(10) 0.206(11) Uiso 1 4 d S . . N805 N 0.3270(7) 0.0399(7) 0.3035(9) 0.045(5) Uiso 0.25 1 d P . . C809 C 0.3372(10) 0.0506(10) 0.3218(12) 0.058(8) Uiso 0.25 1 d P . . C808 C 0.392(2) 0.079(2) 0.313(3) 0.23(4) Uiso 0.25 1 d P . . 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 Cr1 0.0354(7) 0.0354(7) 0.0247(10) 0.000 0.000 -0.0146(8) V1 0.0287(8) 0.0267(8) 0.0208(7) 0.000 0.000 -0.0062(5) V2 0.0379(6) 0.0379(6) 0.0345(8) 0.0043(5) -0.0043(5) -0.0072(6) P1 0.0352(11) 0.0352(11) 0.0433(18) 0.000 0.000 0.000 P2 0.0521(15) 0.0404(13) 0.0304(12) -0.0005(10) 0.000 0.000 P3 0.158(5) 0.158(5) 0.145(8) 0.000 0.000 -0.013(7) C1 0.035(5) 0.036(5) 0.027(4) 0.000 0.000 -0.008(4) C2 0.037(3) 0.037(3) 0.032(5) -0.001(3) 0.001(3) -0.005(4) C3 0.047(3) 0.047(3) 0.030(5) 0.003(3) -0.003(3) -0.003(4) C10 0.033(3) 0.035(3) 0.031(3) 0.001(3) -0.002(2) -0.008(3) C11 0.040(3) 0.031(3) 0.023(3) 0.009(2) 0.003(2) -0.004(3) C12 0.027(3) 0.037(3) 0.027(3) 0.005(2) -0.002(2) -0.008(2) C13 0.043(4) 0.043(4) 0.035(3) -0.003(3) 0.002(3) -0.009(3) C14 0.033(3) 0.051(4) 0.030(3) -0.002(3) -0.001(3) -0.003(3) C15 0.047(4) 0.047(4) 0.035(3) 0.008(3) 0.000(3) 0.010(3) C16 0.031(3) 0.072(5) 0.035(4) 0.010(3) 0.004(3) 0.001(3) C17 0.040(4) 0.061(4) 0.032(3) 0.005(3) -0.007(3) -0.012(3) C18 0.050(4) 0.060(4) 0.038(4) 0.000(3) -0.013(3) -0.005(3) C19 0.035(3) 0.041(3) 0.020(3) -0.003(2) -0.001(2) -0.010(3) C20 0.053(4) 0.052(4) 0.027(3) -0.008(3) -0.002(3) -0.014(3) C21 0.061(4) 0.043(4) 0.035(3) -0.005(3) -0.001(3) -0.019(3) C22 0.051(4) 0.065(5) 0.039(4) 0.012(3) -0.003(3) 0.010(4) C23 0.051(4) 0.040(4) 0.028(3) -0.005(3) 0.008(3) -0.003(3) C24 0.048(4) 0.040(4) 0.042(4) 0.011(3) -0.002(3) -0.010(3) C25 0.036(3) 0.046(4) 0.044(4) 0.001(3) -0.004(3) 0.002(3) C26 0.038(4) 0.043(4) 0.044(4) 0.006(3) -0.006(3) -0.005(3) C27 0.062(6) 0.037(5) 0.048(6) 0.000 0.000 -0.031(5) C28 0.047(4) 0.057(4) 0.045(4) -0.007(3) 0.006(3) -0.015(3) C29 0.056(4) 0.050(4) 0.037(4) 0.007(3) 0.012(3) 0.012(3) C30 0.036(4) 0.075(5) 0.043(4) 0.024(4) -0.005(3) 0.001(3) C31 0.070(4) 0.070(4) 0.031(5) 0.006(3) -0.006(3) -0.009(6) C32 0.071(5) 0.042(4) 0.083(6) -0.007(4) 0.003(4) -0.008(4) C33 0.040(4) 0.050(4) 0.046(4) 0.003(3) -0.009(3) -0.001(3) C34 0.048(4) 0.069(5) 0.039(4) -0.001(3) -0.005(3) 0.006(4) C35 0.037(4) 0.079(5) 0.048(4) -0.018(4) -0.007(3) -0.002(4) C36 0.063(5) 0.049(4) 0.054(4) -0.011(3) 0.011(4) -0.007(4) C37 0.056(5) 0.054(4) 0.056(4) 0.011(3) 0.006(4) -0.018(3) C38 0.069(5) 0.058(5) 0.066(5) -0.013(4) 0.000(4) -0.006(4) C39 0.058(4) 0.038(4) 0.062(5) 0.006(3) 0.002(4) -0.010(3) N1 0.042(4) 0.035(4) 0.030(4) 0.000 0.000 -0.008(4) N2 0.040(3) 0.040(3) 0.044(4) 0.001(3) -0.001(3) -0.011(3) N3 0.071(4) 0.071(4) 0.039(5) -0.006(3) 0.006(3) 0.005(5) N5 0.030(3) 0.030(3) 0.022(2) 0.0015(19) 0.0005(19) -0.004(2) N6 0.033(4) 0.029(3) 0.018(3) 0.000 0.000 -0.007(3) N7 0.030(3) 0.041(3) 0.028(2) 0.009(2) -0.001(2) -0.005(2) N8 0.044(3) 0.043(3) 0.042(3) 0.001(2) 0.000(2) -0.008(2) N9 0.035(2) 0.035(2) 0.041(4) 0.004(2) -0.004(2) -0.006(3) N10 0.042(3) 0.050(3) 0.033(3) 0.001(2) -0.005(2) -0.008(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 Cr1 C1 2.043(8) . ? Cr1 C1 2.043(9) 31 ? Cr1 C2 2.048(9) 18_556 ? Cr1 C2 2.048(9) . ? Cr1 C3 2.068(10) . ? Cr1 C3 2.068(10) 18_556 ? V1 N1 2.040(7) . ? V1 N6 2.098(6) . ? V1 N7 2.132(5) 18_556 ? V1 N7 2.132(5) . ? V1 N5 2.133(5) 18_556 ? V1 N5 2.133(5) . ? V2 N2 2.076(8) . ? V2 N9 2.100(7) . ? V2 N8 2.140(5) 31 ? V2 N8 2.140(5) . ? V2 N10 2.150(5) 31 ? V2 N10 2.150(5) . ? P1 F2 1.584(9) . ? P1 F1 1.596(4) 3 ? P1 F1 1.596(4) . ? P1 F1 1.596(4) 4 ? P1 F1 1.596(4) 2 ? P1 F3 1.618(10) 4 ? P1 F3 1.618(10) 3 ? P1 F3 1.618(10) 2 ? P1 F3 1.618(10) . ? P2 F6 1.583(5) . ? P2 F6 1.583(5) 6 ? P2 F4 1.585(4) . ? P2 F4 1.585(4) 6 ? P2 F5 1.591(5) 6 ? P2 F5 1.591(5) . ? P3 F9 1.475(18) . ? P3 F10 1.58(2) 31 ? P3 F10 1.58(2) . ? P3 F8 1.63(2) . ? P3 F8 1.63(2) 18_556 ? P3 F7 1.68(3) . ? P4 P4 1.09(3) 18_556 ? P4 F162 1.44(8) . ? P4 F15 1.43(6) . ? P4 F13 1.45(3) . ? P4 F16 1.50(5) . ? P4 F12 1.50(3) . ? P4 F11 1.53(3) . ? P4 F161 1.53(5) . ? P4 F14 1.56(4) . ? P4 F14 2.20(4) 18_556 ? F3 F3 0.47(2) 4 ? F3 F3 0.47(2) 3 ? F3 F3 0.66(3) 2 ? F10 F12 1.76(3) . ? F11 P4 1.53(3) 18_556 ? F12 P4 1.50(3) 18_556 ? F13 P4 1.45(3) 18_556 ? F13 F15 1.74(7) . ? F13 F15 1.74(7) 18_556 ? F14 F161 0.65(6) . ? F14 F162 1.55(9) . ? F14 P4 2.20(4) 18_556 ? F15 F162 1.34(9) . ? F15 F16 1.49(7) . ? F16 F162 1.13(8) . ? C1 N1 1.139(10) . ? C2 N2 1.124(11) . ? C3 N3 1.142(12) . ? C10 N6 1.354(6) . ? C10 C21 1.399(8) . ? C10 C19 1.550(7) . ? C11 N5 1.350(7) . ? C11 C23 1.371(8) . ? C11 C19 1.562(8) . ? C12 N7 1.343(7) . ? C12 C17 1.393(8) . ? C12 C19 1.543(8) . ? C13 N10 1.350(8) . ? C13 C28 1.379(9) . ? C13 C24 1.560(9) . ? C14 N5 1.348(7) . ? C14 C16 1.369(9) . ? C15 N7 1.353(8) . ? C15 C22 1.365(9) . ? C16 C29 1.380(10) . ? C17 C30 1.386(10) . ? C18 C31 1.380(8) . ? C18 C25 1.385(9) . ? C19 C20 1.534(8) . ? C21 C27 1.370(8) . ? C22 C30 1.378(10) . ? C23 C29 1.389(9) . ? C24 C26 1.529(9) . ? C24 C25 1.537(9) 31 ? C24 C37 1.551(9) . ? C25 N9 1.356(7) . ? C25 C24 1.537(9) 31 ? C26 N8 1.358(8) . ? C26 C39 1.401(9) . ? C27 C21 1.370(8) 18_556 ? C28 C35 1.411(10) . ? C31 C18 1.380(8) 31 ? C32 C39 1.361(11) . ? C32 C38 1.366(12) . ? C33 N10 1.329(8) . ? C33 C34 1.367(10) . ? C34 C35 1.331(11) . ? C36 N8 1.334(9) . ? C36 C38 1.400(10) . ? C800 N800 1.163(14) . ? C800 C801 1.420(16) . ? C802 N801 1.14(2) . ? C802 C803 1.37(3) . ? C805 C804 1.55(8) . ? C806 C806 1.03(9) 15_455 ? C806 C807 1.87(5) . ? C806 C807 1.87(5) 18_556 ? N807 C807 1.08(7) . ? N6 C10 1.354(6) 18_556 ? N9 C25 1.356(7) 31 ? C804 N802 1.06(4) . ? F161 F162 0.97(8) . ? O800 O810 1.00(3) 27_455 ? O800 O810 1.00(3) . ? O800 C810 1.49(4) 27_455 ? O800 C810 1.49(4) 2_565 ? O800 C810 1.49(4) . ? O800 C810 1.49(4) 28 ? C810 O810 1.73(4) 27_455 ? C810 O810 1.85(4) . ? C807 C806 1.87(5) 15_455 ? O810 C810 1.73(4) 27_455 ? O810 C810 1.73(4) 28 ? O810 C810 1.85(4) 2_565 ? N805 C809 0.72(3) . ? C808 C808 1.41(16) 31 ? 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 C1 Cr1 C1 174.9(5) . 31 ? C1 Cr1 C2 91.81(18) . 18_556 ? C1 Cr1 C2 91.81(18) 31 18_556 ? C1 Cr1 C2 91.81(18) . . ? C1 Cr1 C2 91.81(18) 31 . ? C2 Cr1 C2 89.9(5) 18_556 . ? C1 Cr1 C3 88.19(18) . . ? C1 Cr1 C3 88.19(18) 31 . ? C2 Cr1 C3 180.0(5) 18_556 . ? C2 Cr1 C3 90.1(3) . . ? C1 Cr1 C3 88.19(18) . 18_556 ? C1 Cr1 C3 88.19(18) 31 18_556 ? C2 Cr1 C3 90.1(3) 18_556 18_556 ? C2 Cr1 C3 180.0(5) . 18_556 ? C3 Cr1 C3 90.0(5) . 18_556 ? N1 V1 N6 179.5(3) . . ? N1 V1 N7 92.64(19) . 18_556 ? N6 V1 N7 87.69(17) . 18_556 ? N1 V1 N7 92.64(19) . . ? N6 V1 N7 87.69(17) . . ? N7 V1 N7 99.3(3) 18_556 . ? N1 V1 N5 92.32(18) . 18_556 ? N6 V1 N5 87.35(17) . 18_556 ? N7 V1 N5 81.10(18) 18_556 18_556 ? N7 V1 N5 175.00(18) . 18_556 ? N1 V1 N5 92.32(18) . . ? N6 V1 N5 87.35(17) . . ? N7 V1 N5 175.00(18) 18_556 . ? N7 V1 N5 81.10(18) . . ? N5 V1 N5 98.1(2) 18_556 . ? N2 V2 N9 176.3(3) . . ? N2 V2 N8 94.8(2) . 31 ? N9 V2 N8 87.6(2) . 31 ? N2 V2 N8 94.8(2) . . ? N9 V2 N8 87.6(2) . . ? N8 V2 N8 97.1(3) 31 . ? N2 V2 N10 90.7(2) . 31 ? N9 V2 N10 86.87(19) . 31 ? N8 V2 N10 81.6(2) 31 31 ? N8 V2 N10 174.4(2) . 31 ? N2 V2 N10 90.7(2) . . ? N9 V2 N10 86.87(19) . . ? N8 V2 N10 174.4(2) 31 . ? N8 V2 N10 81.6(2) . . ? N10 V2 N10 99.1(3) 31 . ? F2 P1 F1 89.43(19) . 3 ? F2 P1 F1 89.43(19) . . ? F1 P1 F1 89.994(4) 3 . ? F2 P1 F1 89.43(19) . 4 ? F1 P1 F1 178.9(4) 3 4 ? F1 P1 F1 89.994(4) . 4 ? F2 P1 F1 89.43(19) . 2 ? F1 P1 F1 89.994(4) 3 2 ? F1 P1 F1 178.9(4) . 2 ? F1 P1 F1 89.994(4) 4 2 ? F2 P1 F3 168.2(5) . 4 ? F1 P1 F3 92(3) 3 4 ? F1 P1 F3 78.9(7) . 4 ? F1 P1 F3 89(3) 4 4 ? F1 P1 F3 102.2(7) 2 4 ? F2 P1 F3 168.2(5) . 3 ? F1 P1 F3 89(3) 3 3 ? F1 P1 F3 102.2(7) . 3 ? F1 P1 F3 92(3) 4 3 ? F1 P1 F3 78.9(7) 2 3 ? F3 P1 F3 23.5(11) 4 3 ? F2 P1 F3 168.2(5) . 2 ? F1 P1 F3 102.2(7) 3 2 ? F1 P1 F3 92(3) . 2 ? F1 P1 F3 78.9(7) 4 2 ? F1 P1 F3 89(3) 2 2 ? F3 P1 F3 16.6(8) 4 2 ? F3 P1 F3 16.6(8) 3 2 ? F2 P1 F3 168.2(5) . . ? F1 P1 F3 78.9(7) 3 . ? F1 P1 F3 89(3) . . ? F1 P1 F3 102.2(7) 4 . ? F1 P1 F3 92(3) 2 . ? F3 P1 F3 16.6(8) 4 . ? F3 P1 F3 16.6(8) 3 . ? F3 P1 F3 23.5(11) 2 . ? F6 P2 F6 92.8(3) . 6 ? F6 P2 F4 89.4(2) . . ? F6 P2 F4 90.3(2) 6 . ? F6 P2 F4 90.3(2) . 6 ? F6 P2 F4 89.4(2) 6 6 ? F4 P2 F4 179.6(3) . 6 ? F6 P2 F5 177.7(3) . 6 ? F6 P2 F5 89.5(2) 6 6 ? F4 P2 F5 90.5(2) . 6 ? F4 P2 F5 89.8(2) 6 6 ? F6 P2 F5 89.5(2) . . ? F6 P2 F5 177.7(3) 6 . ? F4 P2 F5 89.8(2) . . ? F4 P2 F5 90.5(2) 6 . ? F5 P2 F5 88.2(3) 6 . ? F9 P3 F10 95.3(8) . 31 ? F9 P3 F10 95.3(8) . . ? F10 P3 F10 169.4(16) 31 . ? F9 P3 F8 93.4(8) . . ? F10 P3 F8 89.69(10) 31 . ? F10 P3 F8 89.68(10) . . ? F9 P3 F8 93.4(8) . 18_556 ? F10 P3 F8 89.69(10) 31 18_556 ? F10 P3 F8 89.68(10) . 18_556 ? F8 P3 F8 173.2(17) . 18_556 ? F9 P3 F7 179.998(5) . . ? F10 P3 F7 84.7(8) 31 . ? F10 P3 F7 84.7(8) . . ? F8 P3 F7 86.6(8) . . ? F8 P3 F7 86.6(8) 18_556 . ? P4 P4 F162 171(3) 18_556 . ? P4 P4 F15 133(3) 18_556 . ? F162 P4 F15 56(4) . . ? P4 P4 F13 68.0(7) 18_556 . ? F162 P4 F13 119(4) . . ? F15 P4 F13 74(3) . . ? P4 P4 F16 135(2) 18_556 . ? F162 P4 F16 45(3) . . ? F15 P4 F16 61(3) . . ? F13 P4 F16 82(2) . . ? P4 P4 F12 68.8(7) 18_556 . ? F162 P4 F12 113(3) . . ? F15 P4 F12 96(3) . . ? F13 P4 F12 105.8(17) . . ? F16 P4 F12 154(2) . . ? P4 P4 F11 69.1(6) 18_556 . ? F162 P4 F11 103(3) . . ? F15 P4 F11 148(3) . . ? F13 P4 F11 102.2(16) . . ? F16 P4 F11 87(2) . . ? F12 P4 F11 114.4(16) . . ? P4 P4 F161 135(2) 18_556 . ? F162 P4 F161 38(3) . . ? F15 P4 F161 85(3) . . ? F13 P4 F161 157(2) . . ? F16 P4 F161 78(3) . . ? F12 P4 F161 88(2) . . ? F11 P4 F161 89(2) . . ? P4 P4 F14 111.5(15) 18_556 . ? F162 P4 F14 62(3) . . ? F15 P4 F14 105(3) . . ? F13 P4 F14 177(2) . . ? F16 P4 F14 100(3) . . ? F12 P4 F14 71.8(18) . . ? F11 P4 F14 79.8(18) . . ? F161 P4 F14 24(2) . . ? P4 P4 F14 41.2(11) 18_556 18_556 ? F162 P4 F14 132(4) . 18_556 ? F15 P4 F14 150(3) . 18_556 ? F13 P4 F14 109.1(13) . 18_556 ? F16 P4 F14 148(2) . 18_556 ? F12 P4 F14 54.1(14) . 18_556 ? F11 P4 F14 61.0(13) . 18_556 ? F161 P4 F14 94(3) . 18_556 ? F14 P4 F14 70(2) . 18_556 ? F3 F3 F3 90.00(11) 4 3 ? F3 F3 F3 45.00(2) 4 2 ? F3 F3 F3 45.00(6) 3 2 ? F3 F3 P1 81.7(4) 4 . ? F3 F3 P1 81.7(4) 3 . ? F3 F3 P1 78.2(5) 2 . ? P3 F10 F12 175.0(17) . . ? P4 F11 P4 41.7(12) 18_556 . ? P4 F12 P4 42.3(13) 18_556 . ? P4 F12 F10 131.9(19) 18_556 . ? P4 F12 F10 131.9(19) . . ? P4 F13 P4 44.0(14) . 18_556 ? P4 F13 F15 52(2) . . ? P4 F13 F15 92(3) 18_556 . ? P4 F13 F15 92(3) . 18_556 ? P4 F13 F15 52(2) 18_556 18_556 ? F15 F13 F15 121(4) . 18_556 ? F161 F14 F162 20(6) . . ? F161 F14 P4 75(6) . . ? F162 F14 P4 55(3) . . ? F161 F14 P4 103(6) . 18_556 ? F162 F14 P4 82(3) . 18_556 ? P4 F14 P4 27.3(9) . 18_556 ? F162 F15 P4 63(4) . . ? F162 F15 F16 47(4) . . ? P4 F15 F16 62(3) . . ? F162 F15 F13 107(5) . . ? P4 F15 F13 53(2) . . ? F16 F15 F13 73(4) . . ? F162 F16 F15 60(5) . . ? F162 F16 P4 65(5) . . ? F15 F16 P4 57(3) . . ? N1 C1 Cr1 174.3(8) . . ? N2 C2 Cr1 173.3(8) . . ? N3 C3 Cr1 179.1(9) . . ? N6 C10 C21 120.4(5) . . ? N6 C10 C19 118.3(5) . . ? C21 C10 C19 121.3(5) . . ? N5 C11 C23 121.3(5) . . ? N5 C11 C19 117.0(5) . . ? C23 C11 C19 121.7(5) . . ? N7 C12 C17 120.5(6) . . ? N7 C12 C19 117.2(5) . . ? C17 C12 C19 122.2(5) . . ? N10 C13 C28 122.3(6) . . ? N10 C13 C24 116.8(5) . . ? C28 C13 C24 120.7(6) . . ? N5 C14 C16 124.5(6) . . ? N7 C15 C22 123.7(7) . . ? C14 C16 C29 117.4(6) . . ? C30 C17 C12 119.6(6) . . ? C31 C18 C25 120.4(7) . . ? C20 C19 C12 109.6(5) . . ? C20 C19 C10 109.1(5) . . ? C12 C19 C10 109.5(4) . . ? C20 C19 C11 109.0(5) . . ? C12 C19 C11 109.3(4) . . ? C10 C19 C11 110.3(4) . . ? C27 C21 C10 119.0(6) . . ? C15 C22 C30 117.8(7) . . ? C11 C23 C29 120.2(6) . . ? C26 C24 C25 111.4(5) . 31 ? C26 C24 C37 108.5(5) . . ? C25 C24 C37 108.3(5) 31 . ? C26 C24 C13 107.9(5) . . ? C25 C24 C13 110.7(5) 31 . ? C37 C24 C13 110.1(6) . . ? N9 C25 C18 120.0(6) . . ? N9 C25 C24 118.2(5) . 31 ? C18 C25 C24 121.8(6) . 31 ? N8 C26 C39 118.7(6) . . ? N8 C26 C24 117.8(5) . . ? C39 C26 C24 123.4(6) . . ? C21 C27 C21 120.7(8) 18_556 . ? C13 C28 C35 117.8(7) . . ? C16 C29 C23 119.0(6) . . ? C22 C30 C17 119.6(6) . . ? C18 C31 C18 118.5(9) . 31 ? C39 C32 C38 120.1(7) . . ? N10 C33 C34 122.7(7) . . ? C35 C34 C33 120.5(7) . . ? C34 C35 C28 118.8(7) . . ? N8 C36 C38 122.6(7) . . ? C32 C38 C36 117.5(7) . . ? C32 C39 C26 121.0(7) . . ? N800 C800 C801 179.998(3) . . ? N801 C802 C803 166(2) . . ? C806 C806 C807 73.9(15) 15_455 . ? C806 C806 C807 73.9(15) 15_455 18_556 ? C807 C806 C807 146(3) . 18_556 ? C1 N1 V1 172.2(7) . . ? C2 N2 V2 161.6(7) . . ? C14 N5 C11 117.4(5) . . ? C14 N5 V1 122.6(4) . . ? C11 N5 V1 119.9(4) . . ? C10 N6 C10 120.5(7) 18_556 . ? C10 N6 V1 119.7(3) 18_556 . ? C10 N6 V1 119.7(3) . . ? C12 N7 C15 118.7(5) . . ? C12 N7 V1 120.1(4) . . ? C15 N7 V1 121.2(4) . . ? C36 N8 C26 119.9(6) . . ? C36 N8 V2 121.4(5) . . ? C26 N8 V2 118.6(4) . . ? C25 N9 C25 120.6(7) . 31 ? C25 N9 V2 119.6(4) . . ? C25 N9 V2 119.6(4) 31 . ? C33 N10 C13 117.7(6) . . ? C33 N10 V2 122.2(4) . . ? C13 N10 V2 119.7(4) . . ? N802 C804 C805 178(6) . . ? F14 F161 F162 146(10) . . ? F14 F161 P4 80(6) . . ? F162 F161 P4 66(5) . . ? F161 F162 F16 130(9) . . ? F161 F162 F15 119(8) . . ? F16 F162 F15 74(6) . . ? F161 F162 P4 76(6) . . ? F16 F162 P4 70(5) . . ? F15 F162 P4 62(4) . . ? F161 F162 F14 13(4) . . ? F16 F162 F14 121(7) . . ? F15 F162 F14 110(6) . . ? P4 F162 F14 63(3) . . ? O810 O800 O810 180.000(14) 27_455 . ? O810 O800 C810 94.1(15) 27_455 27_455 ? O810 O800 C810 85.9(15) . 27_455 ? O810 O800 C810 85.9(15) 27_455 2_565 ? O810 O800 C810 94.1(15) . 2_565 ? C810 O800 C810 90.3(2) 27_455 2_565 ? O810 O800 C810 85.9(15) 27_455 . ? O810 O800 C810 94.1(15) . . ? C810 O800 C810 90.3(2) 27_455 . ? C810 O800 C810 172(3) 2_565 . ? O810 O800 C810 94.1(15) 27_455 28 ? O810 O800 C810 85.9(15) . 28 ? C810 O800 C810 172(3) 27_455 28 ? C810 O800 C810 90.3(2) 2_565 28 ? C810 O800 C810 90.3(2) . 28 ? O800 C810 O810 35.0(13) . 27_455 ? O800 C810 O810 32.5(11) . . ? O810 C810 O810 68(2) 27_455 . ? N807 C807 C806 155(4) . 15_455 ? N807 C807 C806 155(4) . . ? C806 C807 C806 32(3) 15_455 . ? O800 O810 C810 59.1(16) . 27_455 ? O800 O810 C810 59.1(16) . 28 ? C810 O810 C810 118(3) 27_455 28 ? O800 O810 C810 53.4(15) . . ? C810 O810 C810 72.1(11) 27_455 . ? C810 O810 C810 72.1(11) 28 . ? O800 O810 C810 53.4(15) . 2_565 ? C810 O810 C810 72.1(11) 27_455 2_565 ? C810 O810 C810 72.1(11) 28 2_565 ? C810 O810 C810 107(3) . 2_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.683 _refine_diff_density_min -1.693 _refine_diff_density_rms 0.164 # Attachment '25.cif' data_df93a _database_code_depnum_ccdc_archive 'CCDC 730662' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C135 H100 F28 Mo N33 O0.50 P5 V4' _chemical_formula_weight 3179.03 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4/mcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z+1/2' 'x, -y, -z+1/2' 'y, x, -z+1/2' '-y, -x, -z+1/2' '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' '-x+1/2, y+1/2, -z+1' 'x+1/2, -y+1/2, -z+1' 'y+1/2, x+1/2, -z+1' '-y+1/2, -x+1/2, -z+1' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z-1/2' '-x, y, z-1/2' '-y, -x, z-1/2' 'y, x, z-1/2' '-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' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 33.492(2) _cell_length_b 33.492(2) _cell_length_c 29.015(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 32546(5) _cell_formula_units_Z 8 _cell_measurement_temperature 140 _cell_measurement_reflns_used 6229 _cell_measurement_theta_min 4.440 _cell_measurement_theta_max 37.486 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max .25 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12848 _exptl_absorpt_coefficient_mu 0.432 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.856970 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; It is extremely difficult to obtain high-quality crystals of these compounds owing to the size and charge of the polynuclear coordination clusters. Many crystals were examined in an effort to obtain the best quality data. In situations in which a central cluster is surrounded by anion and solvent disorder, frequently the parameters of goodness of fit and wR2 are less than ideal. We believe the structures reported treat the available data in an appropriate manner, and this has been confirmed by consultation with our departmental crystallographer, Dr. Fred Hollander. ; _diffrn_ambient_temperature 140 _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 SMART CCD' _diffrn_measurement_method \w/2\q-scans _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 63396 _diffrn_reflns_av_R_equivalents 0.0897 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 21.99 _reflns_number_total 5259 _reflns_number_gt 3644 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v6.36' _computing_data_reduction 'Bruker SAINT v6.36' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5259 _refine_ls_number_parameters 464 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1317 _refine_ls_R_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.2883 _refine_ls_wR_factor_gt 0.2711 _refine_ls_goodness_of_fit_ref 2.041 _refine_ls_restrained_S_all 2.041 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.24785(4) 0.25215(4) 0.0000 0.0488(6) Uani 1 4 d S . . V1 V 0.11926(6) 0.16132(6) 0.0000 0.0287(6) Uani 1 2 d S . . V2 V 0.30736(5) 0.19264(5) 0.14926(7) 0.0449(7) Uani 1 2 d S . . P1 P 0.0000 0.0000 0.36685(16) 0.0400(12) Uani 1 4 d S . . P2 P 0.17331(10) 0.0000 0.2500 0.0375(8) Uani 1 2 d S . . P3 P 0.4095(3) 0.0905(3) 0.0000 0.175(5) Uani 1 4 d S . . P5 P 0.3577(10) -0.0293(5) -0.019(4) 0.61(9) Uani 0.25 1 d P . . F1 F -0.04386(17) 0.01927(16) 0.36628(19) 0.0629(15) Uiso 1 1 d . . . F2 F 0.0000 0.0000 0.3122(4) 0.069(3) Uiso 1 4 d S . . F3 F 0.0000 0.0000 0.4208(5) 0.091(4) Uiso 1 4 d S . . F4 F 0.17354(14) 0.04505(15) 0.26762(17) 0.0520(14) Uiso 1 1 d . . . F5 F 0.13950(16) 0.01037(16) 0.21373(18) 0.0606(15) Uiso 1 1 d . . . F6 F 0.20569(18) -0.01097(17) 0.2874(2) 0.0711(17) Uiso 1 1 d . . . F7 F 0.3771(6) 0.1229(6) 0.0000 0.198(10) Uiso 1 4 d S . . F8 F 0.4440(8) 0.0560(8) 0.0000 0.262(14) Uiso 1 4 d S . . F9 F 0.3724(8) 0.0521(9) 0.0000 0.281(11) Uiso 1 2 d S . . F10 F 0.4119(5) 0.0881(5) 0.0545(10) 0.275(11) Uiso 1 2 d S . . F11 F 0.3282(12) -0.0558(13) 0.0000 0.212(15) Uiso 0.50 2 d SP . . F12 F 0.3456(10) 0.0078(11) 0.0000 0.171(11) Uiso 0.50 2 d SP . . F13 F 0.3875(15) -0.0400(14) 0.0000 0.244(18) Uiso 0.50 2 d SP . . F14 F 0.3157(19) -0.0130(19) -0.036(2) 0.23(2) Uiso 0.25 1 d P . . C1 C 0.2000(4) 0.2106(4) 0.0000 0.044(3) Uani 1 2 d S . . C2 C 0.2146(4) 0.2854(4) 0.0522(5) 0.057(4) Uani 1 2 d S . . C3 C 0.2780(3) 0.2220(3) 0.0518(4) 0.044(3) Uani 1 2 d S . . C10 C 0.0470(2) 0.1208(2) 0.0404(3) 0.035(2) Uani 1 1 d . . . C11 C 0.0733(2) 0.1791(2) 0.0877(2) 0.032(2) Uani 1 1 d . . . C12 C 0.1096(2) 0.1136(2) 0.0881(3) 0.034(2) Uani 1 1 d . . . C13 C 0.2336(3) 0.1551(3) 0.1933(3) 0.045(2) Uani 1 1 d . . . C14 C 0.1577(4) 0.0731(3) 0.1261(3) 0.058(3) Uani 1 1 d . . . H14A H 0.1646 0.0555 0.1495 0.070 Uiso 1 1 calc R . . C15 C 0.0681(3) 0.1330(3) 0.0855(3) 0.038(2) Uani 1 1 d . . . C16 C 0.1045(3) 0.2358(3) 0.0595(3) 0.042(2) Uani 1 1 d . . . H16A H 0.1219 0.2471 0.0382 0.051 Uiso 1 1 calc R . . C17 C 0.1201(3) 0.0875(3) 0.1238(3) 0.043(2) Uani 1 1 d . . . H17A H 0.1012 0.0801 0.1457 0.051 Uiso 1 1 calc R . . C18 C 0.0428(3) 0.1196(3) 0.1268(3) 0.049(3) Uani 1 1 d . . . H18A H 0.0393 0.0912 0.1258 0.074 Uiso 1 1 calc R . . H18B H 0.0171 0.1325 0.1255 0.074 Uiso 1 1 calc R . . H18C H 0.0560 0.1269 0.1549 0.074 Uiso 1 1 calc R . . C19 C 0.0553(3) 0.2020(3) 0.1218(3) 0.044(2) Uani 1 1 d . . . H19A H 0.0382 0.1902 0.1432 0.053 Uiso 1 1 calc R . . C20 C 0.3009(3) 0.1501(3) 0.2898(3) 0.062(3) Uani 1 1 d . . . H20A H 0.2850 0.1319 0.3056 0.074 Uiso 1 1 calc R . . C21 C 0.1933(3) 0.1484(3) 0.2008(3) 0.055(3) Uani 1 1 d . . . H21A H 0.1854 0.1273 0.2196 0.066 Uiso 1 1 calc R . . C22 C 0.0114(3) 0.0993(3) 0.0413(3) 0.050(3) Uani 1 1 d . . . H22A H -0.0004 0.0921 0.0691 0.060 Uiso 1 1 calc R . . C23 C 0.1732(3) 0.1098(3) 0.0601(3) 0.051(3) Uani 1 1 d . . . H23A H 0.1919 0.1181 0.0383 0.062 Uiso 1 1 calc R . . C24 C 0.2967(3) 0.1544(3) 0.2421(3) 0.049(2) Uani 1 1 d . . . C25 C 0.3934(3) 0.2125(3) 0.1744(3) 0.053(3) Uani 1 1 d . . . C26 C 0.0886(3) 0.2605(3) 0.0927(3) 0.052(3) Uani 1 1 d . . . H26A H 0.0948 0.2875 0.0941 0.063 Uiso 1 1 calc R . . C27 C 0.2662(3) 0.1290(3) 0.2141(3) 0.052(3) Uani 1 1 d . . . C28 C 0.1768(3) 0.2024(3) 0.1523(3) 0.055(3) Uani 1 1 d . . . H28A H 0.1583 0.2188 0.1376 0.066 Uiso 1 1 calc R . . C29 C 0.1861(3) 0.0843(3) 0.0941(3) 0.063(3) Uani 1 1 d . . . H29A H 0.2123 0.0751 0.0954 0.075 Uiso 1 1 calc R . . C30 C -0.0057(4) 0.0890(4) 0.0000 0.059(4) Uani 1 2 d S . . H30A H -0.0295 0.0747 0.0000 0.071 Uiso 1 2 calc SR . . C31 C 0.4526(4) 0.1961(4) 0.1319(5) 0.093(4) Uani 1 1 d . . . H31A H 0.4802 0.1950 0.1296 0.112 Uiso 1 1 calc R . . C32 C 0.0629(3) 0.2427(3) 0.1239(3) 0.054(3) Uani 1 1 d . . . H32A H 0.0507 0.2582 0.1464 0.064 Uiso 1 1 calc R . . C33 C 0.3278(3) 0.1722(3) 0.3130(4) 0.057(4) Uani 1 2 d S . . H33A H 0.3311 0.1689 0.3446 0.068 Uiso 1 2 calc SR . . C34 C 0.4344(3) 0.2120(3) 0.1707(4) 0.066(3) Uani 1 1 d . . . H34A H 0.4500 0.2224 0.1944 0.080 Uiso 1 1 calc R . . C35 C 0.2175(3) 0.2083(3) 0.1458(3) 0.058(3) Uani 1 1 d . . . H35A H 0.2257 0.2289 0.1265 0.070 Uiso 1 1 calc R . . C36 C 0.1644(3) 0.1726(3) 0.1804(3) 0.060(3) Uani 1 1 d . . . H36A H 0.1374 0.1684 0.1859 0.072 Uiso 1 1 calc R . . C37 C 0.3883(3) 0.1832(4) 0.1028(4) 0.078(4) Uani 1 1 d . . . H37A H 0.3723 0.1736 0.0790 0.093 Uiso 1 1 calc R . . C38 C 0.2477(3) 0.0974(3) 0.2465(3) 0.064(3) Uani 1 1 d . . . H38A H 0.2287 0.0816 0.2298 0.096 Uiso 1 1 calc R . . H38B H 0.2346 0.1106 0.2717 0.096 Uiso 1 1 calc R . . H38C H 0.2685 0.0804 0.2583 0.096 Uiso 1 1 calc R . . C39 C 0.4289(4) 0.1821(4) 0.0971(5) 0.101(5) Uani 1 1 d . . . H39A H 0.4402 0.1721 0.0702 0.121 Uiso 1 1 calc R . . C800 C 0.0884(3) 0.0884(3) 0.2500 0.045(3) Uiso 1 2 d S . . C801 C 0.0584(3) 0.0584(3) 0.2500 0.064(4) Uiso 1 2 d S . . C804 C 0.4729(12) 0.2525(10) 0.0000 0.076(10) Uiso 0.50 2 d SP . . C805 C 0.4986(12) 0.2705(12) 0.0000 0.094(11) Uiso 0.50 2 d SP . . N1 N 0.1715(3) 0.1901(3) 0.0000 0.039(3) Uani 1 2 d S . . N2 N 0.1975(3) 0.3025(3) 0.0793(5) 0.086(4) Uani 1 2 d S . . N3 N 0.2935(3) 0.2065(3) 0.0830(4) 0.049(3) Uani 1 2 d S . . N10 N 0.09665(19) 0.1965(2) 0.0555(2) 0.0324(17) Uani 1 1 d . . . N11 N 0.0640(3) 0.1313(3) 0.0000 0.029(2) Uani 1 2 d S . . N12 N 0.1361(2) 0.12366(19) 0.0559(2) 0.0334(17) Uani 1 1 d . . . N13 N 0.3708(2) 0.1971(2) 0.1401(3) 0.058(2) Uani 1 1 d . . . N14 N 0.3187(2) 0.1813(2) 0.2189(3) 0.042(3) Uani 1 2 d S . . N15 N 0.2454(2) 0.1857(2) 0.1659(2) 0.046(2) Uani 1 1 d . . . N800 N 0.1126(3) 0.1126(3) 0.2500 0.070(4) Uiso 1 2 d S . . N803 N 0.4358(5) 0.2524(5) 0.0000 0.104(5) Uiso 1 2 d S . . N801 N 0.4187(15) 0.0813(15) 0.152(2) 0.25(3) Uiso 0.50 2 d SP . . C802 C 0.4702(8) 0.0298(8) 0.2509(15) 0.238(18) Uiso 1 2 d S . . C803 C 0.5000 0.0000 0.2117(13) 0.133(12) Uiso 1 4 d S . . O800 O 0.5000 0.0000 0.2500 0.165(14) Uiso 1 8 d S . . C806 C 0.3964(7) 0.1036(7) 0.1989(12) 0.187(12) Uiso 1 2 d S . . N810 N 0.0430(8) 0.3288(8) 0.1944(9) 0.108(8) Uiso 0.50 1 d P . . C809 C 0.0550(14) 0.3452(13) 0.1723(17) 0.170(17) Uiso 0.50 1 d P . . 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 0.0574(8) 0.0574(8) 0.0317(9) 0.000 0.000 -0.0311(9) V1 0.0336(12) 0.0349(12) 0.0176(10) 0.000 0.000 -0.0084(9) V2 0.0495(10) 0.0495(10) 0.0356(13) 0.0007(8) -0.0007(8) -0.0155(11) P1 0.0377(17) 0.0377(17) 0.045(3) 0.000 0.000 0.000 P2 0.050(2) 0.037(2) 0.0253(17) 0.0005(14) 0.000 0.000 P3 0.203(9) 0.203(9) 0.119(9) 0.000 0.000 0.007(12) P5 0.22(3) 0.039(10) 1.6(2) 0.09(4) -0.48(8) -0.006(14) C1 0.052(9) 0.057(9) 0.022(7) 0.000 0.000 -0.003(7) C2 0.073(7) 0.073(7) 0.024(8) 0.001(5) -0.001(5) -0.008(8) C3 0.050(6) 0.050(6) 0.032(8) -0.003(5) 0.003(5) -0.027(7) C10 0.035(5) 0.039(5) 0.032(5) -0.002(4) -0.001(4) -0.013(4) C11 0.040(5) 0.039(5) 0.018(4) -0.001(4) 0.000(4) -0.003(4) C12 0.045(6) 0.033(5) 0.024(4) -0.004(4) -0.003(4) -0.010(4) C13 0.047(6) 0.051(6) 0.037(5) -0.006(5) -0.003(5) -0.012(5) C14 0.090(9) 0.043(6) 0.041(6) 0.001(5) -0.024(6) 0.002(6) C15 0.047(6) 0.046(6) 0.022(5) -0.002(4) 0.011(4) -0.015(4) C16 0.066(7) 0.039(6) 0.022(5) 0.002(4) -0.001(4) -0.006(5) C17 0.051(7) 0.046(6) 0.032(5) 0.004(4) -0.003(5) -0.011(5) C18 0.064(7) 0.055(6) 0.028(5) -0.001(4) 0.018(4) -0.019(5) C19 0.048(6) 0.055(7) 0.030(5) -0.005(5) 0.005(4) -0.003(5) C20 0.067(8) 0.075(8) 0.042(6) 0.014(5) 0.004(5) -0.003(6) C21 0.061(8) 0.064(7) 0.040(6) -0.008(5) 0.013(5) -0.022(6) C22 0.054(7) 0.066(7) 0.030(5) -0.002(5) 0.009(5) -0.020(5) C23 0.072(8) 0.058(7) 0.024(5) 0.002(5) -0.006(5) 0.000(5) C24 0.049(6) 0.051(6) 0.048(6) 0.000(5) 0.005(5) -0.003(5) C25 0.047(7) 0.058(7) 0.053(6) -0.004(5) 0.002(5) -0.015(5) C26 0.082(8) 0.043(6) 0.033(5) -0.002(5) -0.012(5) 0.000(5) C27 0.060(7) 0.049(6) 0.046(6) 0.001(5) 0.002(5) -0.019(5) C28 0.053(7) 0.065(7) 0.048(6) 0.002(5) -0.008(5) 0.000(5) C29 0.078(8) 0.070(8) 0.039(6) 0.002(6) -0.008(6) 0.021(6) C30 0.050(9) 0.076(11) 0.052(10) 0.000 0.000 -0.041(8) C31 0.060(9) 0.091(10) 0.127(12) -0.025(9) 0.020(9) -0.012(7) C32 0.065(7) 0.063(8) 0.033(5) -0.015(5) -0.007(5) 0.021(5) C33 0.071(6) 0.071(6) 0.028(7) 0.004(5) -0.004(5) -0.014(8) C34 0.047(7) 0.071(8) 0.081(8) -0.016(6) -0.006(6) -0.013(6) C35 0.058(8) 0.068(7) 0.049(6) 0.006(5) -0.005(5) -0.016(6) C36 0.049(7) 0.089(9) 0.044(6) -0.008(6) -0.002(5) -0.007(6) C37 0.061(8) 0.105(10) 0.067(8) -0.032(7) 0.027(6) -0.024(7) C38 0.076(8) 0.058(7) 0.058(7) 0.011(5) 0.011(6) -0.017(5) C39 0.071(10) 0.122(12) 0.110(11) -0.049(9) 0.027(8) -0.021(8) N1 0.041(7) 0.054(7) 0.022(5) 0.000 0.000 -0.019(6) N2 0.102(7) 0.102(7) 0.054(9) -0.008(6) 0.008(6) 0.009(9) N3 0.053(5) 0.053(5) 0.041(7) -0.003(4) 0.003(4) -0.022(6) N10 0.044(4) 0.034(5) 0.019(3) -0.003(3) 0.000(3) 0.000(3) N11 0.034(6) 0.038(6) 0.014(5) 0.000 0.000 -0.013(4) N12 0.038(5) 0.040(4) 0.023(4) 0.002(3) -0.003(3) 0.001(3) N13 0.055(6) 0.066(6) 0.051(5) -0.010(4) 0.006(4) -0.022(4) N14 0.043(4) 0.043(4) 0.041(6) -0.002(4) 0.002(4) -0.012(5) N15 0.052(5) 0.055(5) 0.033(4) 0.004(4) -0.004(4) -0.014(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 Mo1 C3 2.074(15) . ? Mo1 C3 2.074(15) 18 ? Mo1 C1 2.123(15) . ? Mo1 C1 2.123(15) 31 ? Mo1 C2 2.185(16) . ? Mo1 C2 2.185(16) 18 ? V1 N1 1.999(11) . ? V1 N11 2.105(9) . ? V1 N12 2.130(6) . ? V1 N12 2.130(6) 18 ? V1 N10 2.132(6) 18 ? V1 N10 2.132(6) . ? V2 N3 2.032(12) . ? V2 N14 2.091(10) . ? V2 N15 2.143(8) 31 ? V2 N15 2.143(8) . ? V2 N13 2.146(8) 31 ? V2 N13 2.146(8) . ? P1 F3 1.566(14) . ? P1 F2 1.587(13) . ? P1 F1 1.604(5) 3 ? P1 F1 1.604(5) 4 ? P1 F1 1.604(5) . ? P1 F1 1.604(5) 2 ? P2 F6 1.577(6) . ? P2 F6 1.577(6) 6 ? P2 F5 1.584(6) . ? P2 F5 1.584(6) 6 ? P2 F4 1.593(5) 6 ? P2 F4 1.593(5) . ? P3 F7 1.53(3) . ? P3 F10 1.59(3) 18 ? P3 F10 1.59(3) . ? P3 F8 1.63(4) . ? P3 F9 1.79(3) . ? P3 F9 1.79(3) 31 ? P5 P5 1.1(2) 18 ? P5 F13 1.20(5) . ? P5 F12 1.43(6) . ? P5 F11 1.44(6) . ? P5 F14 1.58(7) . ? P5 F14 2.20(10) 18 ? F9 F12 1.73(4) . ? F11 P5 1.44(6) 18 ? F12 P5 1.43(6) 18 ? F12 F14 1.60(6) 18 ? F12 F14 1.60(6) . ? F13 P5 1.20(5) 18 ? F14 P5 2.20(10) 18 ? C1 N1 1.174(15) . ? C2 N2 1.128(17) . ? C3 N3 1.164(15) . ? C10 N11 1.351(9) . ? C10 C22 1.392(11) . ? C10 C15 1.542(11) . ? C11 N10 1.350(10) . ? C11 C19 1.391(11) . ? C11 C15 1.556(11) . ? C12 N12 1.333(10) . ? C12 C17 1.400(11) . ? C12 C15 1.536(12) . ? C13 N15 1.354(11) . ? C13 C21 1.387(12) . ? C13 C27 1.522(13) . ? C14 C17 1.352(13) . ? C14 C29 1.382(14) . ? C15 C18 1.536(10) . ? C16 N10 1.348(10) . ? C16 C26 1.376(12) . ? C19 C32 1.387(13) . ? C20 C33 1.347(12) . ? C20 C24 1.399(12) . ? C21 C36 1.395(14) . ? C22 C30 1.372(11) . ? C23 N12 1.333(11) . ? C23 C29 1.375(13) . ? C24 N14 1.346(10) . ? C24 C27 1.557(13) . ? C25 N13 1.351(11) . ? C25 C34 1.379(13) . ? C25 C27 1.549(13) 31 ? C26 C32 1.382(13) . ? C27 C38 1.545(12) . ? C27 C25 1.549(13) 31 ? C28 C36 1.353(13) . ? C28 C35 1.390(14) . ? C30 C22 1.372(11) 18 ? C31 C39 1.365(17) . ? C31 C34 1.384(16) . ? C33 C20 1.347(12) 31 ? C35 N15 1.338(12) . ? C37 N13 1.318(12) . ? C37 C39 1.372(16) . ? C800 N800 1.146(15) . ? C800 C801 1.422(19) . ? C804 C805 1.05(4) . ? C804 N803 1.24(4) . ? N11 C10 1.351(9) 18 ? N14 C24 1.346(10) 31 ? N801 C806 1.72(7) . ? C802 O800 1.41(4) . ? C802 C803 1.78(4) 27 ? C802 C803 1.81(4) . ? C802 C802 2.00(6) 27 ? C802 C802 2.00(6) 28_545 ? C803 O800 1.11(4) . ? C803 C802 1.78(4) 27 ? C803 C802 1.78(4) 28_545 ? C803 C802 1.81(4) 2_655 ? O800 C803 1.11(4) 27 ? O800 C802 1.41(4) 28_545 ? O800 C802 1.41(4) 27 ? O800 C802 1.41(4) 2_655 ? N810 C809 0.94(5) . ? 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 C3 Mo1 C3 92.9(7) . 18 ? C3 Mo1 C1 92.8(2) . . ? C3 Mo1 C1 92.8(2) 18 . ? C3 Mo1 C1 92.8(2) . 31 ? C3 Mo1 C1 92.8(2) 18 31 ? C1 Mo1 C1 171.8(7) . 31 ? C3 Mo1 C2 89.6(5) . . ? C3 Mo1 C2 177.4(5) 18 . ? C1 Mo1 C2 87.1(3) . . ? C1 Mo1 C2 87.1(3) 31 . ? C3 Mo1 C2 177.4(5) . 18 ? C3 Mo1 C2 89.6(5) 18 18 ? C1 Mo1 C2 87.1(3) . 18 ? C1 Mo1 C2 87.1(3) 31 18 ? C2 Mo1 C2 87.8(7) . 18 ? N1 V1 N11 179.7(4) . . ? N1 V1 N12 93.1(3) . . ? N11 V1 N12 87.1(2) . . ? N1 V1 N12 93.1(3) . 18 ? N11 V1 N12 87.1(2) . 18 ? N12 V1 N12 99.1(4) . 18 ? N1 V1 N10 92.6(3) . 18 ? N11 V1 N10 87.2(2) . 18 ? N12 V1 N10 174.3(3) . 18 ? N12 V1 N10 81.2(2) 18 18 ? N1 V1 N10 92.6(3) . . ? N11 V1 N10 87.2(2) . . ? N12 V1 N10 81.2(2) . . ? N12 V1 N10 174.3(3) 18 . ? N10 V1 N10 98.0(3) 18 . ? N3 V2 N14 176.0(5) . . ? N3 V2 N15 90.9(3) . 31 ? N14 V2 N15 86.5(3) . 31 ? N3 V2 N15 90.9(3) . . ? N14 V2 N15 86.5(3) . . ? N15 V2 N15 99.2(4) 31 . ? N3 V2 N13 95.4(3) . 31 ? N14 V2 N13 87.3(3) . 31 ? N15 V2 N13 173.6(3) 31 31 ? N15 V2 N13 81.5(3) . 31 ? N3 V2 N13 95.4(3) . . ? N14 V2 N13 87.3(3) . . ? N15 V2 N13 81.5(3) 31 . ? N15 V2 N13 173.6(3) . . ? N13 V2 N13 97.1(4) 31 . ? F3 P1 F2 180.000(2) . . ? F3 P1 F1 90.6(3) . 3 ? F2 P1 F1 89.4(3) . 3 ? F3 P1 F1 90.6(3) . 4 ? F2 P1 F1 89.4(3) . 4 ? F1 P1 F1 178.8(5) 3 4 ? F3 P1 F1 90.6(3) . . ? F2 P1 F1 89.4(3) . . ? F1 P1 F1 89.994(6) 3 . ? F1 P1 F1 89.994(6) 4 . ? F3 P1 F1 90.6(3) . 2 ? F2 P1 F1 89.4(3) . 2 ? F1 P1 F1 89.994(6) 3 2 ? F1 P1 F1 89.994(6) 4 2 ? F1 P1 F1 178.8(5) . 2 ? F6 P2 F6 93.2(5) . 6 ? F6 P2 F5 177.8(3) . . ? F6 P2 F5 89.0(3) 6 . ? F6 P2 F5 89.0(3) . 6 ? F6 P2 F5 177.8(3) 6 6 ? F5 P2 F5 88.8(4) . 6 ? F6 P2 F4 89.8(3) . 6 ? F6 P2 F4 89.8(3) 6 6 ? F5 P2 F4 89.9(3) . 6 ? F5 P2 F4 90.5(3) 6 6 ? F6 P2 F4 89.8(3) . . ? F6 P2 F4 89.8(3) 6 . ? F5 P2 F4 90.5(3) . . ? F5 P2 F4 89.9(3) 6 . ? F4 P2 F4 179.5(4) 6 . ? F7 P3 F10 94.1(11) . 18 ? F7 P3 F10 94.1(11) . . ? F10 P3 F10 172(2) 18 . ? F7 P3 F8 179.999(7) . . ? F10 P3 F8 85.9(11) 18 . ? F10 P3 F8 85.9(11) . . ? F7 P3 F9 91.1(10) . . ? F10 P3 F9 89.93(8) 18 . ? F10 P3 F9 89.93(8) . . ? F8 P3 F9 88.9(10) . . ? F7 P3 F9 91.1(10) . 31 ? F10 P3 F9 89.92(8) 18 31 ? F10 P3 F9 89.92(8) . 31 ? F8 P3 F9 88.9(10) . 31 ? F9 P3 F9 178(2) . 31 ? P5 P5 F13 62(5) 18 . ? P5 P5 F12 67(4) 18 . ? F13 P5 F12 108(5) . . ? P5 P5 F11 67(4) 18 . ? F13 P5 F11 102(5) . . ? F12 P5 F11 101(5) . . ? P5 P5 F14 107(4) 18 . ? F13 P5 F14 169(8) . . ? F12 P5 F14 64(2) . . ? F11 P5 F14 74(3) . . ? P5 P5 F14 43(2) 18 18 ? F13 P5 F14 105(7) . 18 ? F12 P5 F14 47(3) . 18 ? F11 P5 F14 55(4) . 18 ? F14 P5 F14 64(4) . 18 ? F12 F9 P3 167(2) . . ? P5 F11 P5 46(7) . 18 ? P5 F12 P5 47(7) . 18 ? P5 F12 F14 93(4) . 18 ? P5 F12 F14 63(3) 18 18 ? P5 F12 F14 63(3) . . ? P5 F12 F14 93(4) 18 . ? F14 F12 F14 80(5) 18 . ? P5 F12 F9 127(3) . . ? P5 F12 F9 127(3) 18 . ? F14 F12 F9 134(3) 18 . ? F14 F12 F9 134(3) . . ? P5 F13 P5 56(10) 18 . ? P5 F14 F12 53(3) . . ? P5 F14 P5 29(5) . 18 ? F12 F14 P5 40(2) . 18 ? N1 C1 Mo1 175.0(12) . . ? N2 C2 Mo1 179.7(17) . . ? N3 C3 Mo1 175.4(12) . . ? N11 C10 C22 120.8(8) . . ? N11 C10 C15 118.2(7) . . ? C22 C10 C15 121.0(7) . . ? N10 C11 C19 120.5(8) . . ? N10 C11 C15 117.6(6) . . ? C19 C11 C15 121.9(7) . . ? N12 C12 C17 120.6(8) . . ? N12 C12 C15 117.4(7) . . ? C17 C12 C15 121.9(7) . . ? N15 C13 C21 119.9(9) . . ? N15 C13 C27 117.3(8) . . ? C21 C13 C27 122.8(9) . . ? C17 C14 C29 120.9(9) . . ? C12 C15 C18 109.7(7) . . ? C12 C15 C10 110.1(6) . . ? C18 C15 C10 109.3(7) . . ? C12 C15 C11 108.6(6) . . ? C18 C15 C11 108.6(7) . . ? C10 C15 C11 110.4(7) . . ? N10 C16 C26 125.0(9) . . ? C14 C17 C12 119.5(9) . . ? C32 C19 C11 119.4(8) . . ? C33 C20 C24 120.3(10) . . ? C13 C21 C36 121.0(10) . . ? C30 C22 C10 118.1(9) . . ? N12 C23 C29 125.1(9) . . ? N14 C24 C20 120.5(9) . . ? N14 C24 C27 117.7(8) . . ? C20 C24 C27 121.8(8) . . ? N13 C25 C34 119.8(9) . . ? N13 C25 C27 116.8(8) . 31 ? C34 C25 C27 123.1(9) . 31 ? C16 C26 C32 116.0(9) . . ? C13 C27 C38 110.4(8) . . ? C13 C27 C25 108.3(7) . 31 ? C38 C27 C25 107.8(8) . 31 ? C13 C27 C24 111.2(8) . . ? C38 C27 C24 108.5(8) . . ? C25 C27 C24 110.5(8) 31 . ? C36 C28 C35 119.1(10) . . ? C23 C29 C14 115.7(10) . . ? C22 C30 C22 121.6(12) . 18 ? C39 C31 C34 118.6(12) . . ? C26 C32 C19 120.7(8) . . ? C20 C33 C20 119.2(13) 31 . ? C25 C34 C31 120.3(10) . . ? N15 C35 C28 123.1(9) . . ? C28 C36 C21 118.2(10) . . ? N13 C37 C39 123.3(11) . . ? C31 C39 C37 118.6(12) . . ? N800 C800 C801 180.0(9) . . ? C805 C804 N803 145(4) . . ? C1 N1 V1 172.9(11) . . ? C3 N3 V2 159.9(11) . . ? C16 N10 C11 118.2(7) . . ? C16 N10 V1 122.4(5) . . ? C11 N10 V1 119.4(5) . . ? C10 N11 C10 120.5(9) 18 . ? C10 N11 V1 119.7(5) 18 . ? C10 N11 V1 119.7(5) . . ? C23 N12 C12 118.0(7) . . ? C23 N12 V1 121.5(6) . . ? C12 N12 V1 120.5(6) . . ? C37 N13 C25 119.4(9) . . ? C37 N13 V2 121.1(7) . . ? C25 N13 V2 119.3(6) . . ? C24 N14 C24 119.1(11) . 31 ? C24 N14 V2 120.3(5) . . ? C24 N14 V2 120.3(5) 31 . ? C35 N15 C13 118.7(8) . . ? C35 N15 V2 121.1(6) . . ? C13 N15 V2 119.8(6) . . ? O800 C802 C803 38.6(16) . 27 ? O800 C802 C803 37.8(15) . . ? C803 C802 C803 76(3) 27 . ? O800 C802 C802 44.99(4) . 27 ? C803 C802 C802 57.0(15) 27 27 ? C803 C802 C802 55.4(15) . 27 ? O800 C802 C802 44.99(4) . 28_545 ? C803 C802 C802 57.0(15) 27 28_545 ? C803 C802 C802 55.4(15) . 28_545 ? C802 C802 C802 89.96(14) 27 28_545 ? O800 C803 C802 52.5(18) . 27 ? O800 C803 C802 52.5(18) . 28_545 ? C802 C803 C802 105(4) 27 28_545 ? O800 C803 C802 51.2(18) . 2_655 ? C802 C803 C802 67.6(15) 27 2_655 ? C802 C803 C802 67.6(15) 28_545 2_655 ? O800 C803 C802 51.2(18) . . ? C802 C803 C802 67.6(15) 27 . ? C802 C803 C802 67.6(15) 28_545 . ? C802 C803 C802 102(4) 2_655 . ? C803 O800 C803 180.000(8) . 27 ? C803 O800 C802 88.9(17) . 28_545 ? C803 O800 C802 91.1(17) 27 28_545 ? C803 O800 C802 88.9(17) . 27 ? C803 O800 C802 91.1(17) 27 27 ? C802 O800 C802 178(3) 28_545 27 ? C803 O800 C802 91.1(17) . 2_655 ? C803 O800 C802 88.9(17) 27 2_655 ? C802 O800 C802 90.02(7) 28_545 2_655 ? C802 O800 C802 90.02(7) 27 2_655 ? C803 O800 C802 91.1(17) . . ? C803 O800 C802 88.9(17) 27 . ? C802 O800 C802 90.02(7) 28_545 . ? C802 O800 C802 90.02(7) 27 . ? C802 O800 C802 178(3) 2_655 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 21.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.429 _refine_diff_density_min -1.296 _refine_diff_density_rms 0.158