Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'J.Chem. Soc. Dalton Trans' loop_ _publ_author_name 'S. M. O. Quintal' 'H. I. S. Nogueira' 'H. M. Carapuca' 'V. Felix' 'M. G. B. Drew' _publ_contact_author_name 'Dr Helena I S Nogueira' _publ_contact_author_email HELENA@DQ.UA.PT _publ_contact_author_address ; Department of Chemistry University of Aveiro Aveiro 3810-193 PORTUGAL ; _publ_section_title ; Polinuclear molybdenum and tungsten complexes of 3-hydroxypicolinic acid and the crystal structures of (nBu4N)2[Mo4O12(picOH)2] and (nHex4N)2[Mo2O6(picOH)2] ; _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1997) SHELX-97, University of Gottingen, Germany. Spek, A.L., (1999) A Multiple Crystallographic tool, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #------------------------- data section of block --------------------------- #==BEGIN data_compound1 _database_code_CSD 162915 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety (n-Bu4N)2[Mo4O12(picOH)2] _chemical_formula_sum 'C44 H80 Mo4 N4 O18' _chemical_formula_weight 1336.88 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 Orthorhombic _symmetry_space_group_name_H-M P22121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, y+1/2, -z+1/2' '-x, -y+1/2, z+1/2' _cell_length_a 8.758(11) _cell_length_b 17.540(23) _cell_length_c 18.560(25) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2851(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.927 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '92 frames at 5^o intervals, counting time 5 min.' _diffrn_standards_number all _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8475 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4826 _reflns_number_gt 3776 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+6.7780P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0014(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(2) _refine_ls_number_reflns 4826 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1291 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.34442(7) 0.94007(3) 0.43413(3) 0.03696(18) Uani 1 d . . . Mo2 Mo 0.32573(8) 0.83136(3) 0.57359(4) 0.0432(2) Uani 1 d . . . O1 O 0.3600(6) 0.9518(3) 0.5457(2) 0.0425(11) Uani 1 d . . . O3 O 0.1973(8) 0.9444(3) 0.3753(3) 0.0650(17) Uani 1 d . . . O2 O 0.2928(6) 0.8410(3) 0.4738(3) 0.0492(13) Uani 1 d . . . O4 O 0.5144(7) 0.8133(3) 0.5825(4) 0.0647(17) Uani 1 d . . . O5 O 0.2384(7) 0.7460(3) 0.5907(4) 0.0641(17) Uani 1 d . . . O6 O 0.5046(9) 0.9222(4) 0.3876(4) 0.078(2) Uani 1 d . . . N1 N 0.0793(8) 0.8853(4) 0.5886(3) 0.0486(16) Uani 1 d . . . C2 C 0.0555(10) 0.9119(4) 0.6564(5) 0.053(2) Uani 1 d . . . C3 C -0.0844(12) 0.9410(5) 0.6784(6) 0.068(3) Uani 1 d . . . C4 C -0.1993(12) 0.9447(7) 0.6300(8) 0.087(3) Uani 1 d . . . H4 H -0.2939 0.9641 0.6436 0.104 Uiso 1 calc R . . C5 C -0.1762(11) 0.9199(5) 0.5607(7) 0.078(3) Uani 1 d . . . H5 H -0.2548 0.9224 0.5270 0.094 Uiso 1 calc R . . C6 C -0.0330(10) 0.8906(5) 0.5410(5) 0.059(2) Uani 1 d . . . H6 H -0.0166 0.8746 0.4938 0.071 Uiso 1 calc R . . C21 C 0.1913(12) 0.9057(5) 0.7052(5) 0.059(2) Uani 1 d . . . O22 O 0.3115(8) 0.8753(3) 0.6774(3) 0.0576(15) Uani 1 d . . . O23 O 0.1805(10) 0.9273(4) 0.7684(3) 0.086(2) Uani 1 d . . . O31 O -0.1017(10) 0.9658(5) 0.7475(5) 0.106(3) Uani 1 d . . . H31 H -0.0219 0.9592 0.7697 0.127 Uiso 1 calc R . . N21 N 0.2179(7) 0.8164(3) 0.1978(4) 0.0422(15) Uani 1 d . . . C31 C 0.3247(9) 0.8851(4) 0.2003(4) 0.0465(18) Uani 1 d . . . H31A H 0.2680 0.9297 0.1849 0.056 Uiso 1 calc R . . H31B H 0.3548 0.8933 0.2500 0.056 Uiso 1 calc R . . C32 C 0.4673(10) 0.8792(5) 0.1551(5) 0.059(2) Uani 1 d . . . H32A H 0.5301 0.8375 0.1722 0.071 Uiso 1 calc R . . H32B H 0.4399 0.8690 0.1053 0.071 Uiso 1 calc R . . C33 C 0.5551(11) 0.9525(6) 0.1596(6) 0.076(3) Uani 1 d . . . H33A H 0.4873 0.9944 0.1476 0.091 Uiso 1 calc R . . H33B H 0.5892 0.9598 0.2088 0.091 Uiso 1 calc R . . C34 C 0.6906(14) 0.9553(7) 0.1107(7) 0.096(4) Uani 1 d . . . H34A H 0.6607 0.9399 0.0630 0.115 Uiso 1 calc R . . H34B H 0.7680 0.9213 0.1283 0.115 Uiso 1 calc R . . H34C H 0.7301 1.0063 0.1092 0.115 Uiso 1 calc R . . C41 C 0.1755(11) 0.7967(4) 0.1209(4) 0.0468(19) Uani 1 d . . . H41A H 0.1010 0.7558 0.1220 0.056 Uiso 1 calc R . . H41B H 0.2658 0.7772 0.0969 0.056 Uiso 1 calc R . . C42 C 0.1104(10) 0.8616(5) 0.0752(5) 0.059(2) Uani 1 d . . . H42A H 0.0160 0.8798 0.0964 0.070 Uiso 1 calc R . . H42B H 0.1823 0.9036 0.0739 0.070 Uiso 1 calc R . . C43 C 0.0805(12) 0.8331(6) -0.0010(5) 0.073(3) Uani 1 d . . . H43A H 0.1745 0.8125 -0.0208 0.088 Uiso 1 calc R . . H43B H 0.0062 0.7922 0.0007 0.088 Uiso 1 calc R . . C44 C 0.0229(17) 0.8945(6) -0.0496(4) 0.119(5) Uani 1 d . . . H44A H -0.0770 0.9101 -0.0342 0.142 Uiso 1 calc R . . H44B H 0.0175 0.8756 -0.0981 0.142 Uiso 1 calc R . . H44C H 0.0911 0.9373 -0.0479 0.142 Uiso 1 calc R . . C51 C 0.0769(10) 0.8377(4) 0.2410(4) 0.054(2) Uani 1 d R . . H51A H 0.0288 0.8811 0.2178 0.065 Uiso 1 calc R . . H51B H 0.1098 0.8543 0.2884 0.065 Uiso 1 calc R . . C52 C -0.0436(11) 0.7758(7) 0.2507(6) 0.075(3) Uani 1 d . . . H52A H -0.0003 0.7338 0.2779 0.090 Uiso 1 calc R . . H52B H -0.0741 0.7566 0.2039 0.090 Uiso 1 calc R . . C53 C -0.1834(14) 0.8067(7) 0.2903(6) 0.087(3) Uani 1 d . . . H53A H -0.2213 0.8509 0.2644 0.104 Uiso 1 calc R . . H53B H -0.2629 0.7681 0.2893 0.104 Uiso 1 calc R . . C54 C -0.1561(17) 0.8278(8) 0.3632(6) 0.105(4) Uani 1 d . . . H54A H -0.0923 0.7902 0.3857 0.126 Uiso 1 calc R . . H54B H -0.2515 0.8309 0.3884 0.126 Uiso 1 calc R . . H54C H -0.1061 0.8765 0.3645 0.126 Uiso 1 calc R . . C61 C 0.2932(10) 0.7459(4) 0.2294(4) 0.051(2) Uani 1 d . . . H61A H 0.3829 0.7344 0.2007 0.061 Uiso 1 calc R . . H61B H 0.2231 0.7035 0.2240 0.061 Uiso 1 calc R . . C62 C 0.3416(12) 0.7499(4) 0.3080(4) 0.057(2) Uani 1 d . . . H62A H 0.2540 0.7622 0.3378 0.068 Uiso 1 calc R . . H62B H 0.4171 0.7898 0.3142 0.068 Uiso 1 calc R . . C63 C 0.4092(13) 0.6733(6) 0.3318(5) 0.072(3) Uani 1 d . . . H63A H 0.3329 0.6337 0.3260 0.086 Uiso 1 calc R . . H63B H 0.4952 0.6607 0.3011 0.086 Uiso 1 calc R . . C64 C 0.4611(17) 0.6750(6) 0.4090(6) 0.102(4) Uani 1 d . . . H64A H 0.5485 0.7077 0.4134 0.123 Uiso 1 calc R . . H64B H 0.4879 0.6244 0.4241 0.123 Uiso 1 calc R . . H64C H 0.3801 0.6940 0.4389 0.123 Uiso 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 0.0440(4) 0.0298(3) 0.0371(3) -0.0026(3) 0.0046(3) 0.0030(3) Mo2 0.0457(4) 0.0330(3) 0.0508(4) 0.0085(3) -0.0060(3) 0.0013(3) O1 0.053(3) 0.036(3) 0.039(2) -0.003(2) -0.004(2) 0.001(2) O3 0.099(5) 0.041(3) 0.055(3) -0.003(3) -0.033(3) -0.005(4) O2 0.064(4) 0.028(2) 0.056(3) -0.006(2) 0.000(3) -0.002(2) O4 0.051(4) 0.063(4) 0.080(5) 0.015(3) -0.008(3) 0.011(3) O5 0.070(4) 0.047(3) 0.075(4) 0.013(3) 0.001(3) -0.006(3) O6 0.087(5) 0.055(4) 0.091(5) -0.010(3) 0.049(4) 0.004(3) N1 0.049(4) 0.048(4) 0.048(4) 0.003(3) -0.005(3) -0.002(3) C2 0.046(5) 0.038(4) 0.076(6) 0.013(4) 0.016(4) -0.009(3) C3 0.072(7) 0.044(5) 0.087(7) 0.001(5) 0.032(5) -0.007(5) C4 0.043(7) 0.064(6) 0.154(11) 0.020(8) 0.027(6) 0.002(5) C5 0.049(6) 0.065(6) 0.121(9) 0.022(6) -0.010(6) 0.000(4) C6 0.055(6) 0.042(5) 0.081(6) 0.013(4) -0.012(4) -0.009(4) C21 0.069(7) 0.045(5) 0.063(6) 0.009(4) 0.006(5) -0.014(4) O22 0.056(4) 0.061(4) 0.055(3) 0.009(3) -0.004(3) -0.006(3) O23 0.126(7) 0.092(5) 0.040(3) -0.009(3) 0.010(4) -0.020(5) O31 0.117(7) 0.090(6) 0.111(6) -0.006(5) 0.053(5) 0.010(5) N21 0.039(4) 0.043(4) 0.046(4) -0.009(3) 0.001(3) -0.001(3) C31 0.044(5) 0.036(4) 0.060(5) -0.010(3) 0.004(4) -0.003(4) C32 0.050(6) 0.050(5) 0.076(6) -0.011(4) 0.011(4) -0.008(4) C33 0.060(6) 0.063(6) 0.106(8) -0.013(6) 0.017(5) -0.019(5) C34 0.091(9) 0.083(8) 0.114(9) -0.008(7) 0.009(7) -0.028(7) C41 0.054(5) 0.044(4) 0.043(4) -0.014(3) -0.003(4) -0.002(4) C42 0.059(5) 0.065(5) 0.053(5) -0.014(4) -0.006(4) 0.010(4) C43 0.085(7) 0.083(7) 0.053(5) 0.001(5) -0.006(5) 0.000(6) C44 0.159(14) 0.120(11) 0.077(9) 0.010(7) -0.041(9) 0.036(10) C51 0.060(5) 0.054(5) 0.048(5) -0.010(4) 0.008(4) -0.003(4) C52 0.061(7) 0.102(8) 0.061(6) -0.030(5) 0.027(5) -0.029(5) C53 0.068(8) 0.103(9) 0.090(8) 0.004(7) 0.013(7) -0.008(6) C54 0.105(10) 0.117(10) 0.091(9) -0.001(8) 0.027(8) 0.016(10) C61 0.061(6) 0.039(4) 0.053(5) -0.003(4) 0.001(4) 0.001(4) C62 0.070(6) 0.042(4) 0.058(5) -0.001(4) -0.005(5) 0.010(4) C63 0.082(7) 0.062(6) 0.072(7) 0.006(5) 0.001(5) 0.010(5) C64 0.159(13) 0.069(7) 0.080(8) 0.002(6) -0.040(8) 0.041(8) _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 O6 1.677(7) . ? Mo1 O3 1.691(6) . ? Mo1 O1 1.937(5) 2_576 ? Mo1 O2 1.940(5) . ? Mo1 O1 2.086(5) . ? Mo1 Mo2 3.219(3) . ? Mo2 O4 1.691(6) . ? Mo2 O5 1.711(6) . ? Mo2 O2 1.882(6) . ? Mo2 O22 2.078(6) . ? Mo2 O1 2.196(6) . ? Mo2 N1 2.372(7) . ? O1 Mo1 1.937(5) 2_576 ? N1 C6 1.325(10) . ? N1 C2 1.358(11) . ? C2 C3 1.389(13) . ? C2 C21 1.499(13) . ? C3 C4 1.351(15) . ? C3 O31 1.363(12) . ? C4 C5 1.374(16) . ? C5 C6 1.404(14) . ? C21 O23 1.236(11) . ? C21 O22 1.288(11) . ? N21 C41 1.515(9) . ? N21 C61 1.519(10) . ? N21 C51 1.519(9) . ? N21 C31 1.526(9) . ? C31 C32 1.509(11) . ? C32 C33 1.501(12) . ? C33 C34 1.495(14) . ? C41 C42 1.529(11) . ? C42 C43 1.523(12) . ? C43 C44 1.493(12) . ? C51 C52 1.524(12) . ? C52 C53 1.527(14) . ? C53 C54 1.423(16) . ? C61 C62 1.522(11) . ? C62 C63 1.533(12) . ? C63 C64 1.503(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Mo1 O3 108.2(4) . . ? O6 Mo1 O1 102.9(3) . 2_576 ? O3 Mo1 O1 97.7(3) . 2_576 ? O6 Mo1 O2 102.9(3) . . ? O3 Mo1 O2 96.2(3) . . ? O1 Mo1 O2 145.0(2) 2_576 . ? O6 Mo1 O1 118.4(3) . . ? O3 Mo1 O1 133.4(3) . . ? O1 Mo1 O1 73.0(2) 2_576 . ? O2 Mo1 O1 74.2(2) . . ? O4 Mo2 O5 104.8(3) . . ? O4 Mo2 O2 105.2(3) . . ? O5 Mo2 O2 101.1(3) . . ? O4 Mo2 O22 92.1(3) . . ? O5 Mo2 O22 97.2(3) . . ? O2 Mo2 O22 150.4(2) . . ? O4 Mo2 O1 94.0(2) . . ? O5 Mo2 O1 161.2(3) . . ? O2 Mo2 O1 72.70(19) . . ? O22 Mo2 O1 82.5(2) . . ? O4 Mo2 N1 162.2(3) . . ? O5 Mo2 N1 85.4(3) . . ? O2 Mo2 N1 86.6(2) . . ? O22 Mo2 N1 71.9(2) . . ? O1 Mo2 N1 76.6(2) . . ? Mo1 O1 Mo1 106.5(2) 2_576 . ? Mo1 O1 Mo2 152.4(3) 2_576 . ? Mo1 O1 Mo2 97.45(19) . . ? Mo2 O2 Mo1 114.7(3) . . ? C6 N1 C2 118.6(8) . . ? C6 N1 Mo2 128.7(6) . . ? C2 N1 Mo2 112.7(5) . . ? N1 C2 C3 122.3(9) . . ? N1 C2 C21 114.4(7) . . ? C3 C2 C21 123.3(9) . . ? C4 C3 O31 121.9(10) . . ? C4 C3 C2 118.6(10) . . ? O31 C3 C2 119.5(10) . . ? C3 C4 C5 119.9(10) . . ? C4 C5 C6 119.4(10) . . ? N1 C6 C5 121.0(10) . . ? O23 C21 O22 124.8(9) . . ? O23 C21 C2 119.3(9) . . ? O22 C21 C2 115.9(8) . . ? C21 O22 Mo2 125.0(6) . . ? C41 N21 C61 106.5(6) . . ? C41 N21 C51 110.7(6) . . ? C61 N21 C51 110.5(6) . . ? C41 N21 C31 111.1(6) . . ? C61 N21 C31 111.4(6) . . ? C51 N21 C31 106.7(6) . . ? C32 C31 N21 115.9(6) . . ? C33 C32 C31 109.5(7) . . ? C34 C33 C32 113.6(9) . . ? N21 C41 C42 116.3(6) . . ? C43 C42 C41 109.6(7) . . ? C44 C43 C42 112.5(8) . . ? N21 C51 C52 116.7(6) . . ? C51 C52 C53 111.1(9) . . ? C54 C53 C52 114.5(11) . . ? N21 C61 C62 117.0(6) . . ? C61 C62 C63 110.1(7) . . ? C64 C63 C62 111.9(8) . . ? _refine_diff_density_max 1.524 _refine_diff_density_min -0.859 _refine_diff_density_rms 0.106 #==END data_compound2 _database_code_CSD 162916 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety (n-Hex4N)2[Mo2O6(picOH)2] _chemical_formula_sum 'C60 H112 Mo2 N4 O12' _chemical_formula_weight 1273.42 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.233(21) _cell_length_b 15.273(23) _cell_length_c 16.196(27) _cell_angle_alpha 90.00 _cell_angle_beta 115.70(1) _cell_angle_gamma 90.00 _cell_volume 3395(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.426 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6003 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.86 _reflns_number_total 6003 _reflns_number_gt 4325 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+3.4009P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0068(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6003 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1634 _refine_ls_wR_factor_gt 0.1416 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.125 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo 0.41629(3) 0.06366(2) 0.44042(2) 0.04516(18) Uani 1 d . . . O1 O 0.5569(2) 0.05166(19) 0.55989(19) 0.0470(7) Uani 1 d . . . O2 O 0.3519(3) 0.0750(2) 0.5037(2) 0.0641(9) Uani 1 d . . . O3 O 0.3315(2) 0.0821(2) 0.3299(2) 0.0633(9) Uani 1 d . . . N1 N 0.5291(3) 0.0934(3) 0.3753(3) 0.0519(9) Uani 1 d . . . C2 C 0.5523(4) 0.1786(3) 0.3793(3) 0.0612(13) Uani 1 d . . . C3 C 0.6080(5) 0.2115(4) 0.3357(5) 0.0856(19) Uani 1 d . . . C4 C 0.6381(5) 0.1528(5) 0.2882(5) 0.095(2) Uani 1 d . . . H4 H 0.6734 0.1723 0.2572 0.114 Uiso 1 calc R . . C5 C 0.6161(4) 0.0673(4) 0.2866(4) 0.0758(16) Uani 1 d . . . H5 H 0.6377 0.0275 0.2560 0.091 Uiso 1 calc R . . C6 C 0.5614(4) 0.0389(4) 0.3306(3) 0.0600(13) Uani 1 d . . . H6 H 0.5466 -0.0203 0.3289 0.072 Uiso 1 calc R . . O23 O 0.5316(4) 0.3151(3) 0.4355(3) 0.0977(14) Uani 1 d . . . C21 C 0.5118(4) 0.2357(3) 0.4288(4) 0.0642(14) Uani 1 d . . . O22 O 0.4592(3) 0.1997(2) 0.4621(2) 0.0613(9) Uani 1 d . . . O31 O 0.6304(4) 0.2972(3) 0.3409(4) 0.1231(19) Uani 1 d . . . H31 H 0.6073 0.3226 0.3715 0.148 Uiso 1 calc R . . N21 N 0.6863(3) 0.1969(3) 0.7863(3) 0.0543(10) Uani 1 d . . . C31 C 0.5967(4) 0.2361(4) 0.7065(3) 0.0650(14) Uani 1 d . . . H31A H 0.5785 0.1979 0.6538 0.078 Uiso 1 calc R . . H31B H 0.5430 0.2367 0.7235 0.078 Uiso 1 calc R . . C32 C 0.6102(4) 0.3281(4) 0.6783(4) 0.0854(18) Uani 1 d . . . H32A H 0.6427 0.3250 0.6384 0.102 Uiso 1 calc R . . H32B H 0.6516 0.3612 0.7324 0.102 Uiso 1 calc R . . C33 C 0.5131(5) 0.3760(5) 0.6286(5) 0.098(2) Uani 1 d . . . H33A H 0.5225 0.4253 0.5954 0.118 Uiso 1 calc R . . H33B H 0.4666 0.3366 0.5841 0.118 Uiso 1 calc R . . C34 C 0.4711(6) 0.4090(5) 0.6912(5) 0.105(2) Uani 1 d . . . H34A H 0.4568 0.3591 0.7204 0.126 Uiso 1 calc R . . H34B H 0.5202 0.4440 0.7391 0.126 Uiso 1 calc R . . C35 C 0.3808(7) 0.4627(5) 0.6459(6) 0.116(3) Uani 1 d . . . H35A H 0.3968 0.5159 0.6227 0.139 Uiso 1 calc R . . H35B H 0.3343 0.4303 0.5938 0.139 Uiso 1 calc R . . C36 C 0.3336(8) 0.4870(6) 0.7052(6) 0.134(3) Uani 1 d . . . H36A H 0.3201 0.4351 0.7310 0.161 Uiso 1 calc R . . H36B H 0.2739 0.5174 0.6696 0.161 Uiso 1 calc R . . H36C H 0.3763 0.5244 0.7536 0.161 Uiso 1 calc R . . C41 C 0.7102(4) 0.2485(4) 0.8738(3) 0.0605(13) Uani 1 d . . . H41A H 0.7202 0.3093 0.8627 0.073 Uiso 1 calc R . . H41B H 0.7712 0.2267 0.9209 0.073 Uiso 1 calc R . . C42 C 0.6335(4) 0.2448(4) 0.9104(4) 0.0714(15) Uani 1 d . . . H42A H 0.6291 0.1854 0.9295 0.086 Uiso 1 calc R . . H42B H 0.5705 0.2603 0.8617 0.086 Uiso 1 calc R . . C43 C 0.6573(4) 0.3070(4) 0.9916(4) 0.0717(15) Uani 1 d . . . H43A H 0.6720 0.3643 0.9750 0.086 Uiso 1 calc R . . H43B H 0.5998 0.3129 1.0026 0.086 Uiso 1 calc R . . C44 C 0.7405(4) 0.2788(4) 1.0787(4) 0.0724(15) Uani 1 d . . . H44A H 0.8003 0.2811 1.0711 0.087 Uiso 1 calc R . . H44B H 0.7305 0.2187 1.0918 0.087 Uiso 1 calc R . . C45 C 0.7513(5) 0.3376(4) 1.1601(4) 0.0865(18) Uani 1 d . . . H45A H 0.7554 0.3982 1.1444 0.104 Uiso 1 calc R . . H45B H 0.6936 0.3314 1.1707 0.104 Uiso 1 calc R . . C46 C 0.8390(5) 0.3156(5) 1.2462(5) 0.111(2) Uani 1 d . . . H46A H 0.8374 0.2547 1.2601 0.133 Uiso 1 calc R . . H46B H 0.8393 0.3505 1.2956 0.133 Uiso 1 calc R . . H46C H 0.8967 0.3275 1.2382 0.133 Uiso 1 calc R . . C51 C 0.6615(4) 0.1028(3) 0.7963(3) 0.0602(13) Uani 1 d . . . H51A H 0.6443 0.0732 0.7384 0.072 Uiso 1 calc R . . H51B H 0.6042 0.1025 0.8080 0.072 Uiso 1 calc R . . C52 C 0.7412(4) 0.0501(4) 0.8715(4) 0.0729(15) Uani 1 d . . . H52A H 0.7942 0.0401 0.8546 0.087 Uiso 1 calc R . . H52B H 0.7667 0.0835 0.9280 0.087 Uiso 1 calc R . . C53 C 0.7040(5) -0.0373(4) 0.8875(4) 0.0815(17) Uani 1 d . . . H53A H 0.6728 -0.0675 0.8292 0.098 Uiso 1 calc R . . H53B H 0.7596 -0.0723 0.9270 0.098 Uiso 1 calc R . . C54 C 0.6336(5) -0.0335(4) 0.9295(4) 0.0769(16) Uani 1 d . . . H54A H 0.5750 -0.0035 0.8876 0.092 Uiso 1 calc R . . H54B H 0.6623 0.0008 0.9854 0.092 Uiso 1 calc R . . C55 C 0.6058(7) -0.1223(5) 0.9515(6) 0.111(3) Uani 1 d . . . H55A H 0.5824 -0.1579 0.8965 0.134 Uiso 1 calc R . . H55B H 0.6639 -0.1502 0.9969 0.134 Uiso 1 calc R . . C56 C 0.5294(7) -0.1212(6) 0.9868(7) 0.140(3) Uani 1 d . . . H56A H 0.5530 -0.0885 1.0429 0.168 Uiso 1 calc R . . H56B H 0.5154 -0.1802 0.9979 0.168 Uiso 1 calc R . . H56C H 0.4712 -0.0944 0.9422 0.168 Uiso 1 calc R . . C61 C 0.7760(4) 0.2017(4) 0.7671(3) 0.0621(13) Uani 1 d . . . H61A H 0.8306 0.1751 0.8180 0.075 Uiso 1 calc R . . H61B H 0.7920 0.2627 0.7642 0.075 Uiso 1 calc R . . C62 C 0.7632(4) 0.1564(5) 0.6784(4) 0.087(2) Uani 1 d . . . H62A H 0.7406 0.0970 0.6781 0.104 Uiso 1 calc R . . H62B H 0.7138 0.1871 0.6266 0.104 Uiso 1 calc R . . C63 C 0.8552(5) 0.1542(5) 0.6677(4) 0.0877(19) Uani 1 d . . . H63A H 0.9017 0.1161 0.7141 0.105 Uiso 1 calc R . . H63B H 0.8830 0.2125 0.6768 0.105 Uiso 1 calc R . . C64 C 0.8365(5) 0.1200(6) 0.5698(5) 0.106(2) Uani 1 d . . . H64A H 0.8059 0.0629 0.5606 0.127 Uiso 1 calc R . . H64B H 0.7910 0.1593 0.5243 0.127 Uiso 1 calc R . . C65 C 0.9226(6) 0.1129(7) 0.5540(6) 0.130(3) Uani 1 d . . . H65A H 0.9664 0.0702 0.5961 0.156 Uiso 1 calc R . . H65B H 0.9559 0.1689 0.5665 0.156 Uiso 1 calc R . . C66 C 0.8990(6) 0.0859(7) 0.4575(5) 0.129(3) Uani 1 d . . . H66A H 0.8533 0.0383 0.4398 0.155 Uiso 1 calc R . . H66B H 0.9576 0.0675 0.4540 0.155 Uiso 1 calc R . . H66C H 0.8711 0.1346 0.4170 0.155 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0418(2) 0.0427(3) 0.0444(3) -0.00102(17) 0.01256(18) 0.00559(17) O1 0.0428(15) 0.0407(17) 0.0470(17) -0.0030(13) 0.0095(14) -0.0034(13) O2 0.059(2) 0.071(2) 0.069(2) 0.0021(17) 0.0343(18) 0.0155(17) O3 0.056(2) 0.065(2) 0.057(2) 0.0015(16) 0.0125(17) 0.0133(17) N1 0.048(2) 0.051(2) 0.051(2) 0.0026(18) 0.0158(18) -0.0008(18) C2 0.054(3) 0.055(3) 0.061(3) 0.017(2) 0.013(2) -0.003(2) C3 0.080(4) 0.073(4) 0.105(5) 0.021(4) 0.041(4) -0.010(3) C4 0.087(5) 0.099(5) 0.121(6) 0.032(4) 0.065(4) 0.004(4) C5 0.075(4) 0.081(4) 0.082(4) 0.014(3) 0.044(3) 0.012(3) C6 0.058(3) 0.066(3) 0.055(3) 0.008(2) 0.024(3) 0.007(3) O23 0.134(4) 0.046(2) 0.109(3) -0.003(2) 0.049(3) -0.010(2) C21 0.076(3) 0.043(3) 0.058(3) 0.004(2) 0.014(3) 0.001(3) O22 0.072(2) 0.0442(19) 0.060(2) 0.0000(16) 0.0221(18) 0.0079(17) O31 0.138(4) 0.073(3) 0.175(5) 0.023(3) 0.083(4) -0.025(3) N21 0.052(2) 0.061(2) 0.051(2) -0.0158(19) 0.0240(18) -0.0211(19) C31 0.054(3) 0.081(4) 0.055(3) -0.008(3) 0.019(2) -0.015(3) C32 0.071(4) 0.094(5) 0.079(4) 0.012(3) 0.021(3) -0.016(3) C33 0.108(5) 0.096(5) 0.093(5) 0.007(4) 0.045(4) -0.002(4) C34 0.138(7) 0.085(5) 0.092(5) 0.004(4) 0.050(5) 0.006(5) C35 0.148(8) 0.098(6) 0.112(6) 0.016(5) 0.066(6) 0.022(5) C36 0.180(9) 0.116(7) 0.125(7) 0.008(5) 0.085(7) 0.028(6) C41 0.062(3) 0.066(3) 0.054(3) -0.021(2) 0.025(2) -0.017(3) C42 0.070(3) 0.090(4) 0.064(3) -0.017(3) 0.038(3) -0.018(3) C43 0.079(4) 0.074(4) 0.072(3) -0.010(3) 0.042(3) -0.003(3) C44 0.074(3) 0.067(4) 0.081(4) -0.006(3) 0.037(3) -0.003(3) C45 0.103(5) 0.082(4) 0.072(4) -0.010(3) 0.036(4) 0.010(4) C46 0.112(6) 0.125(6) 0.083(5) -0.011(4) 0.030(4) 0.009(5) C51 0.062(3) 0.063(3) 0.062(3) -0.013(3) 0.033(3) -0.018(3) C52 0.068(3) 0.078(4) 0.073(4) -0.003(3) 0.031(3) -0.007(3) C53 0.100(5) 0.071(4) 0.078(4) -0.002(3) 0.043(4) 0.003(3) C54 0.091(4) 0.071(4) 0.076(4) -0.001(3) 0.043(4) -0.007(3) C55 0.144(7) 0.082(5) 0.125(6) 0.014(4) 0.074(6) -0.010(5) C56 0.167(9) 0.129(8) 0.152(8) 0.036(6) 0.095(7) -0.024(6) C61 0.053(3) 0.077(4) 0.063(3) -0.021(3) 0.031(2) -0.024(3) C62 0.080(4) 0.119(5) 0.078(4) -0.048(4) 0.051(3) -0.043(4) C63 0.093(4) 0.095(5) 0.089(4) -0.015(4) 0.052(4) -0.009(4) C64 0.095(5) 0.122(6) 0.124(6) -0.035(5) 0.070(5) -0.020(5) C65 0.118(6) 0.163(9) 0.128(7) -0.030(6) 0.071(6) 0.001(6) C66 0.122(7) 0.180(9) 0.095(6) -0.040(6) 0.056(5) -0.001(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 Mo O2 1.707(4) . ? Mo O3 1.716(4) . ? Mo O1 1.808(4) 3_656 ? Mo O22 2.161(5) . ? Mo O1 2.184(4) . ? Mo N1 2.418(5) . ? Mo Mo 3.121(3) 3_656 ? O1 Mo 1.808(4) 3_656 ? N1 C6 1.329(7) . ? N1 C2 1.342(7) . ? C2 C3 1.411(8) . ? C2 C21 1.489(8) . ? C3 O31 1.345(8) . ? C3 C4 1.384(10) . ? C4 C5 1.344(9) . ? C5 C6 1.381(8) . ? O23 C21 1.242(7) . ? C21 O22 1.268(6) . ? N21 C51 1.513(7) . ? N21 C41 1.521(6) . ? N21 C61 1.529(6) . ? N21 C31 1.536(6) . ? C31 C32 1.519(8) . ? C32 C33 1.529(9) . ? C33 C34 1.502(10) . ? C34 C35 1.492(11) . ? C35 C36 1.475(11) . ? C41 C42 1.525(7) . ? C42 C43 1.533(7) . ? C43 C44 1.493(8) . ? C44 C45 1.545(8) . ? C45 C46 1.492(9) . ? C51 C52 1.524(8) . ? C52 C53 1.516(8) . ? C53 C54 1.500(8) . ? C54 C55 1.508(9) . ? C55 C56 1.503(10) . ? C61 C62 1.529(7) . ? C62 C63 1.485(8) . ? C63 C64 1.574(9) . ? C64 C65 1.445(10) . ? C65 C66 1.501(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 Mo O3 103.9(2) . . ? O2 Mo O1 106.85(16) . 3_656 ? O3 Mo O1 103.05(15) . 3_656 ? O2 Mo O22 90.97(16) . . ? O3 Mo O22 92.81(15) . . ? O1 Mo O22 152.17(15) 3_656 . ? O2 Mo O1 94.3(2) . . ? O3 Mo O1 160.55(15) . . ? O1 Mo O1 77.58(13) 3_656 . ? O22 Mo O1 79.96(12) . . ? O2 Mo N1 160.92(16) . . ? O3 Mo N1 82.5(2) . . ? O1 Mo N1 88.73(15) 3_656 . ? O22 Mo N1 70.60(14) . . ? O1 Mo N1 78.03(18) . . ? Mo O1 Mo 102.42(13) 3_656 . ? C6 N1 C2 118.8(5) . . ? C6 N1 Mo 128.3(4) . . ? C2 N1 Mo 112.5(3) . . ? N1 C2 C3 121.6(6) . . ? N1 C2 C21 115.6(5) . . ? C3 C2 C21 122.7(5) . . ? O31 C3 C4 121.9(6) . . ? O31 C3 C2 120.5(7) . . ? C4 C3 C2 117.6(6) . . ? C5 C4 C3 120.0(6) . . ? C4 C5 C6 119.8(6) . . ? N1 C6 C5 122.2(5) . . ? O23 C21 O22 124.1(6) . . ? O23 C21 C2 118.5(6) . . ? O22 C21 C2 117.4(5) . . ? C21 O22 Mo 123.4(3) . . ? C51 N21 C41 111.2(4) . . ? C51 N21 C61 110.7(4) . . ? C41 N21 C61 106.9(3) . . ? C51 N21 C31 106.8(4) . . ? C41 N21 C31 110.4(4) . . ? C61 N21 C31 110.9(4) . . ? C32 C31 N21 115.3(4) . . ? C31 C32 C33 112.1(5) . . ? C34 C33 C32 113.8(6) . . ? C35 C34 C33 115.1(7) . . ? C36 C35 C34 115.0(7) . . ? N21 C41 C42 115.4(4) . . ? C41 C42 C43 112.0(4) . . ? C44 C43 C42 114.8(5) . . ? C43 C44 C45 111.8(5) . . ? C46 C45 C44 112.8(6) . . ? N21 C51 C52 116.0(4) . . ? C53 C52 C51 112.0(5) . . ? C54 C53 C52 115.9(5) . . ? C53 C54 C55 113.6(6) . . ? C56 C55 C54 115.0(7) . . ? N21 C61 C62 114.1(4) . . ? C63 C62 C61 112.2(5) . . ? C62 C63 C64 110.9(5) . . ? C65 C64 C63 115.0(6) . . ? C64 C65 C66 112.3(8) . . ? _refine_diff_density_max 0.625 _refine_diff_density_min -0.960 _refine_diff_density_rms 0.087 #==END