Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name _publ_author_address 'Heinze, Katja' ; Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; _publ_contact_author_name 'Dr. Katja Heinze' _publ_contact_author_address ; Dr. Katja Heinze Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; _publ_contact_author_phone '049 6221 54-6238' _publ_contact_author_fax '049 6221 54-5707' _publ_contact_author_email 'katja@sun0.urz.uni-heidelberg.de' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Patterns of hydrogen bonding in organometallic crystals ; #============================================================================== data_ka221 _database_code_CSD 168307 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H10 Mo N2 O5' _chemical_formula_weight 406.20 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 monoklin _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 9.0560(18) _cell_length_b 24.644(5) _cell_length_c 7.0910(14) _cell_angle_alpha 90.00 _cell_angle_beta 108.93(3) _cell_angle_gamma 90.00 _cell_volume 1497.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_type 'experimentell' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _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 'NONIUS KAPPA CCD' _diffrn_measurement_method 'O-Scan ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3781 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.1058 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 30.07 _reflns_number_total 2765 _reflns_number_gt 1860 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0000P)^2^+8.6592P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2765 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1158 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.85143(7) 0.11463(2) 0.10658(9) 0.01993(18) Uani 1 1 d . . . O1 O 0.3131(7) 0.3368(2) -0.1275(9) 0.0342(14) Uani 1 1 d . . . O13 O 1.1668(6) 0.0580(2) 0.1405(8) 0.0373(14) Uani 1 1 d . . . O14 O 0.7746(6) 0.0741(2) -0.3385(8) 0.0398(14) Uani 1 1 d . . . O15 O 0.9541(6) 0.2209(2) -0.0595(8) 0.0329(13) Uani 1 1 d . . . O16 O 0.9942(6) 0.1615(2) 0.5506(8) 0.0384(14) Uani 1 1 d . . . N1 N 0.6047(6) 0.1361(2) 0.0915(8) 0.0191(12) Uani 1 1 d . . . N2 N 0.7522(6) 0.0422(2) 0.2097(8) 0.0192(13) Uani 1 1 d . . . C1 C 0.5267(8) 0.1872(3) 0.0297(10) 0.0209(16) Uani 1 1 d . . . C2 C 0.6092(8) 0.2349(3) 0.0834(10) 0.0221(16) Uani 1 1 d . . . H2 H 0.7153 0.2336 0.1549 0.019(6) Uiso 1 1 calc R . . C3 C 0.5365(8) 0.2846(3) 0.0324(10) 0.0243(16) Uani 1 1 d . . . H3 H 0.5920 0.3166 0.0735 0.019(6) Uiso 1 1 calc R . . C4 C 0.3795(8) 0.2862(3) -0.0807(10) 0.0240(16) Uani 1 1 d . . . C5 C 0.2976(8) 0.2391(3) -0.1411(10) 0.0243(16) Uani 1 1 d . . . H5 H 0.1930 0.2404 -0.2196 0.019(6) Uiso 1 1 calc R . . C6 C 0.3705(8) 0.1894(3) -0.0852(10) 0.0239(17) Uani 1 1 d . . . H6 H 0.3144 0.1575 -0.1251 0.019(6) Uiso 1 1 calc R . . C7 C 0.5276(8) 0.0979(3) 0.1422(10) 0.0206(16) Uani 1 1 d . . . C8 C 0.6015(8) 0.0456(3) 0.2072(10) 0.0214(16) Uani 1 1 d . . . C9 C 0.5240(8) 0.0039(3) 0.2674(10) 0.0228(16) Uani 1 1 d . . . H9 H 0.4208 0.0079 0.2631 0.019(6) Uiso 1 1 calc R . . C10 C 0.6042(8) -0.0439(3) 0.3339(11) 0.0276(18) Uani 1 1 d . . . H10 H 0.5562 -0.0726 0.3764 0.019(6) Uiso 1 1 calc R . . C11 C 0.7543(8) -0.0481(3) 0.3360(11) 0.0281(18) Uani 1 1 d . . . H11 H 0.8099 -0.0799 0.3800 0.019(6) Uiso 1 1 calc R . . C12 C 0.8237(8) -0.0058(3) 0.2740(11) 0.0259(17) Uani 1 1 d . . . H12 H 0.9262 -0.0101 0.2758 0.019(6) Uiso 1 1 calc R . . C13 C 1.0520(8) 0.0802(3) 0.1334(11) 0.0247(16) Uani 1 1 d . . . C14 C 0.7924(8) 0.0873(3) -0.1773(12) 0.0244(17) Uani 1 1 d . . . C15 C 0.9163(8) 0.1816(3) 0.0034(11) 0.0226(16) Uani 1 1 d . . . C16 C 0.9373(8) 0.1450(3) 0.3942(12) 0.0254(17) Uani 1 1 d . . . H1 H 0.223(12) 0.331(5) -0.195(16) 0.10(4) Uiso 1 1 d . . . H7 H 0.418(8) 0.102(3) 0.142(9) 0.026(19) Uiso 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 0.0171(3) 0.0169(3) 0.0251(4) -0.0015(3) 0.0059(3) -0.0003(3) O1 0.031(3) 0.022(3) 0.050(4) 0.007(3) 0.014(3) 0.009(2) O13 0.025(3) 0.034(3) 0.053(4) -0.006(3) 0.013(3) 0.006(2) O14 0.051(4) 0.041(4) 0.030(4) -0.006(3) 0.017(3) -0.013(3) O15 0.034(3) 0.022(3) 0.042(3) 0.003(2) 0.012(3) -0.002(2) O16 0.043(3) 0.039(3) 0.027(3) -0.008(3) 0.003(3) 0.001(3) N1 0.020(3) 0.018(3) 0.015(3) -0.002(2) -0.001(3) -0.002(2) N2 0.017(3) 0.020(3) 0.018(3) -0.004(2) 0.002(3) 0.002(2) C1 0.022(4) 0.019(4) 0.021(4) 0.003(3) 0.006(3) 0.003(3) C2 0.024(4) 0.019(4) 0.023(4) -0.004(3) 0.008(3) -0.004(3) C3 0.032(4) 0.017(4) 0.027(4) 0.001(3) 0.013(4) -0.005(3) C4 0.026(4) 0.024(4) 0.023(4) 0.003(3) 0.009(3) 0.002(3) C5 0.017(4) 0.029(4) 0.027(5) 0.002(3) 0.008(3) 0.000(3) C6 0.024(4) 0.021(4) 0.026(4) -0.004(3) 0.007(3) -0.004(3) C7 0.019(4) 0.024(4) 0.016(4) -0.002(3) 0.003(3) -0.002(3) C8 0.021(4) 0.021(4) 0.018(4) 0.001(3) 0.000(3) -0.001(3) C9 0.019(4) 0.029(4) 0.023(4) -0.001(3) 0.011(3) -0.002(3) C10 0.028(4) 0.019(4) 0.036(5) 0.011(3) 0.010(4) -0.005(3) C11 0.030(4) 0.013(3) 0.034(5) 0.002(3) 0.002(4) 0.003(3) C12 0.025(4) 0.018(4) 0.036(5) -0.005(3) 0.012(4) 0.008(3) C13 0.033(4) 0.018(4) 0.025(4) -0.001(3) 0.013(4) -0.004(3) C14 0.017(4) 0.020(4) 0.033(5) 0.002(3) 0.004(4) -0.005(3) C15 0.021(4) 0.015(3) 0.029(5) -0.002(3) 0.004(3) 0.001(3) C16 0.027(4) 0.015(4) 0.037(5) 0.004(3) 0.013(4) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C13 1.957(7) . ? Mo1 C15 1.971(7) . ? Mo1 C14 2.024(8) . ? Mo1 C16 2.072(8) . ? Mo1 N2 2.226(6) . ? Mo1 N1 2.265(5) . ? O1 C4 1.377(8) . ? O1 H1 0.81(10) . ? O13 C13 1.161(8) . ? O14 C14 1.148(8) . ? O15 C15 1.163(8) . ? O16 C16 1.136(8) . ? N1 C7 1.291(8) . ? N1 C1 1.440(8) . ? N2 C12 1.354(8) . ? N2 C8 1.361(8) . ? C1 C2 1.380(9) . ? C1 C6 1.385(9) . ? C2 C3 1.383(9) . ? C2 H2 0.9300 . ? C3 C4 1.388(9) . ? C3 H3 0.9300 . ? C4 C5 1.370(9) . ? C5 C6 1.387(9) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.456(9) . ? C7 H7 1.00(7) . ? C8 C9 1.388(9) . ? C9 C10 1.383(9) . ? C9 H9 0.9300 . ? C10 C11 1.359(9) . ? C10 H10 0.9300 . ? C11 C12 1.363(10) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? 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 C13 Mo1 C15 91.2(3) . . ? C13 Mo1 C14 83.6(3) . . ? C15 Mo1 C14 85.6(3) . . ? C13 Mo1 C16 91.2(3) . . ? C15 Mo1 C16 90.1(3) . . ? C14 Mo1 C16 173.2(3) . . ? C13 Mo1 N2 94.6(2) . . ? C15 Mo1 N2 173.9(2) . . ? C14 Mo1 N2 93.2(2) . . ? C16 Mo1 N2 91.7(2) . . ? C13 Mo1 N1 167.4(2) . . ? C15 Mo1 N1 101.3(2) . . ? C14 Mo1 N1 95.3(2) . . ? C16 Mo1 N1 90.7(2) . . ? N2 Mo1 N1 72.87(19) . . ? C4 O1 H1 106(8) . . ? C7 N1 C1 117.8(6) . . ? C7 N1 Mo1 115.5(4) . . ? C1 N1 Mo1 126.7(4) . . ? C12 N2 C8 115.3(6) . . ? C12 N2 Mo1 127.6(4) . . ? C8 N2 Mo1 117.1(4) . . ? C2 C1 C6 119.1(6) . . ? C2 C1 N1 119.5(6) . . ? C6 C1 N1 121.4(6) . . ? C1 C2 C3 120.9(6) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C2 C3 C4 119.2(6) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 O1 122.8(6) . . ? C5 C4 C3 120.4(6) . . ? O1 C4 C3 116.8(6) . . ? C4 C5 C6 120.0(6) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C5 120.3(6) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.8 . . ? N1 C7 C8 119.9(6) . . ? N1 C7 H7 123(4) . . ? C8 C7 H7 117(4) . . ? N2 C8 C9 123.7(6) . . ? N2 C8 C7 114.5(6) . . ? C9 C8 C7 121.7(6) . . ? C10 C9 C8 118.2(6) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C11 C10 C9 118.8(6) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 120.2(6) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? N2 C12 C11 123.8(6) . . ? N2 C12 H12 118.1 . . ? C11 C12 H12 118.1 . . ? O13 C13 Mo1 176.3(6) . . ? O14 C14 Mo1 172.3(6) . . ? O15 C15 Mo1 179.3(7) . . ? O16 C16 Mo1 175.4(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 Mo1 N1 C7 5.5(14) . . . . ? C15 Mo1 N1 C7 176.7(5) . . . . ? C14 Mo1 N1 C7 90.1(5) . . . . ? C16 Mo1 N1 C7 -93.1(5) . . . . ? N2 Mo1 N1 C7 -1.6(5) . . . . ? C13 Mo1 N1 C1 -173.8(11) . . . . ? C15 Mo1 N1 C1 -2.5(6) . . . . ? C14 Mo1 N1 C1 -89.1(5) . . . . ? C16 Mo1 N1 C1 87.7(5) . . . . ? N2 Mo1 N1 C1 179.2(5) . . . . ? C13 Mo1 N2 C12 2.7(6) . . . . ? C15 Mo1 N2 C12 165(2) . . . . ? C14 Mo1 N2 C12 86.6(6) . . . . ? C16 Mo1 N2 C12 -88.6(6) . . . . ? N1 Mo1 N2 C12 -178.8(6) . . . . ? C13 Mo1 N2 C8 -176.6(5) . . . . ? C15 Mo1 N2 C8 -14(2) . . . . ? C14 Mo1 N2 C8 -92.7(5) . . . . ? C16 Mo1 N2 C8 92.1(5) . . . . ? N1 Mo1 N2 C8 1.9(5) . . . . ? C7 N1 C1 C2 142.3(7) . . . . ? Mo1 N1 C1 C2 -38.4(8) . . . . ? C7 N1 C1 C6 -38.6(9) . . . . ? Mo1 N1 C1 C6 140.6(5) . . . . ? C6 C1 C2 C3 3.2(10) . . . . ? N1 C1 C2 C3 -177.7(6) . . . . ? C1 C2 C3 C4 -2.4(10) . . . . ? C2 C3 C4 C5 0.0(11) . . . . ? C2 C3 C4 O1 -179.9(6) . . . . ? O1 C4 C5 C6 -178.6(6) . . . . ? C3 C4 C5 C6 1.5(10) . . . . ? C2 C1 C6 C5 -1.6(10) . . . . ? N1 C1 C6 C5 179.3(6) . . . . ? C4 C5 C6 C1 -0.7(10) . . . . ? C1 N1 C7 C8 -179.5(6) . . . . ? Mo1 N1 C7 C8 1.1(8) . . . . ? C12 N2 C8 C9 0.7(10) . . . . ? Mo1 N2 C8 C9 -179.8(5) . . . . ? C12 N2 C8 C7 178.6(6) . . . . ? Mo1 N2 C8 C7 -2.0(7) . . . . ? N1 C7 C8 N2 0.5(9) . . . . ? N1 C7 C8 C9 178.5(7) . . . . ? N2 C8 C9 C10 0.0(10) . . . . ? C7 C8 C9 C10 -177.7(6) . . . . ? C8 C9 C10 C11 -0.5(10) . . . . ? C9 C10 C11 C12 0.2(11) . . . . ? C8 N2 C12 C11 -1.1(10) . . . . ? Mo1 N2 C12 C11 179.5(5) . . . . ? C10 C11 C12 N2 0.7(11) . . . . ? C15 Mo1 C13 O13 -107(10) . . . . ? C14 Mo1 C13 O13 -22(10) . . . . ? C16 Mo1 C13 O13 162(10) . . . . ? N2 Mo1 C13 O13 71(10) . . . . ? N1 Mo1 C13 O13 64(10) . . . . ? C13 Mo1 C14 O14 -47(5) . . . . ? C15 Mo1 C14 O14 44(5) . . . . ? C16 Mo1 C14 O14 -7(6) . . . . ? N2 Mo1 C14 O14 -142(5) . . . . ? N1 Mo1 C14 O14 145(5) . . . . ? C13 Mo1 C15 O15 89(50) . . . . ? C14 Mo1 C15 O15 5(50) . . . . ? C16 Mo1 C15 O15 -180(100) . . . . ? N2 Mo1 C15 O15 -74(51) . . . . ? N1 Mo1 C15 O15 -89(50) . . . . ? C13 Mo1 C16 O16 25(7) . . . . ? C15 Mo1 C16 O16 -66(7) . . . . ? C14 Mo1 C16 O16 -15(9) . . . . ? N2 Mo1 C16 O16 120(7) . . . . ? N1 Mo1 C16 O16 -167(7) . . . . ? _diffrn_measured_fraction_theta_max 0.632 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.632 _refine_diff_density_max 1.550 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.135 #===END # 1. SUBMISSION DETAILS #============================================================================== data_ka237 _database_code_CSD 168308 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22.80 H25.60 Mo N2 O5.95' _chemical_formula_weight 518.79 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 monoklin _symmetry_space_group_name_H-M I2/a (Nr. loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 22.991(5) _cell_length_b 7.9050(16) _cell_length_c 27.559(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.70(3) _cell_angle_gamma 90.00 _cell_volume 4991.8(17) _cell_formula_units_Z 8 _cell_measurement_temperature 200 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 0.563 _exptl_absorpt_correction_type 'experimentell' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _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 'NONIUS KAPPA CCD' _diffrn_measurement_method 'O-Scan ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22486 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.87 _reflns_number_total 5935 _reflns_number_gt 4072 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1051P)^2^+2.5858P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5935 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1835 _refine_ls_wR_factor_gt 0.1653 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.466415(18) 0.27750(5) 0.607189(14) 0.03643(16) Uani 1 1 d . . . O1 O 0.20447(18) -0.1382(6) 0.64288(18) 0.0632(11) Uani 1 1 d . . . O13 O 0.53095(18) 0.6117(5) 0.63884(14) 0.0652(11) Uani 1 1 d . . . O14 O 0.41359(18) 0.5027(4) 0.52282(13) 0.0588(10) Uani 1 1 d . . . O15 O 0.36407(17) 0.4132(4) 0.66332(13) 0.0502(9) Uani 1 1 d . . . O16 O 0.51255(14) 0.1214(4) 0.66884(12) 0.0455(8) Uani 1 1 d . . . N1 N 0.42698(16) 0.0216(4) 0.58950(13) 0.0360(8) Uani 1 1 d . . . N2 N 0.53228(17) 0.1268(5) 0.56758(13) 0.0394(9) Uani 1 1 d . . . C1 C 0.3703(2) -0.0302(5) 0.60172(17) 0.0397(10) Uani 1 1 d . . . C2 C 0.3224(2) 0.0818(6) 0.59148(19) 0.0420(11) Uani 1 1 d . . . C3 C 0.2678(2) 0.0398(6) 0.60459(19) 0.0470(12) Uani 1 1 d . . . C4 C 0.2600(2) -0.1094(7) 0.6294(2) 0.0507(13) Uani 1 1 d . . . C5 C 0.3065(2) -0.2204(6) 0.6396(2) 0.0471(12) Uani 1 1 d . . . C6 C 0.3606(2) -0.1819(6) 0.62600(19) 0.0434(11) Uani 1 1 d . . . C7 C 0.4607(2) -0.0888(6) 0.57328(16) 0.0358(10) Uani 1 1 d . . . C8 C 0.5191(2) -0.0408(6) 0.56130(16) 0.0406(10) Uani 1 1 d . . . C9 C 0.5573(2) -0.1557(7) 0.54320(17) 0.0472(12) Uani 1 1 d . . . C10 C 0.6107(3) -0.1007(8) 0.53129(19) 0.0526(14) Uani 1 1 d . . . C11 C 0.6250(2) 0.0656(9) 0.53666(19) 0.0570(15) Uani 1 1 d . . . C12 C 0.5847(2) 0.1769(8) 0.55455(18) 0.0508(13) Uani 1 1 d . . . C13 C 0.5088(2) 0.4823(7) 0.62680(18) 0.0478(12) Uani 1 1 d . . . C14 C 0.4334(2) 0.4126(5) 0.55386(18) 0.0417(11) Uani 1 1 d . . . C15 C 0.4032(2) 0.3636(5) 0.64274(17) 0.0396(11) Uani 1 1 d . . . C16 C 0.4859(2) 0.0184(7) 0.70345(19) 0.0522(13) Uani 1 1 d . . . H16A H 0.4694 -0.0826 0.6878 0.102(9) Uiso 1 1 calc R . . H16B H 0.4548 0.0804 0.7172 0.102(9) Uiso 1 1 calc R . . C17 C 0.5308(3) -0.0272(11) 0.7415(3) 0.082(2) Uani 1 1 d . . . H17A H 0.5434 -0.1429 0.7372 0.102(9) Uiso 1 1 calc R . . H17B H 0.5158 -0.0171 0.7733 0.102(9) Uiso 1 1 calc R . . C18 C 0.5806(3) 0.0928(8) 0.7372(2) 0.0569(14) Uani 1 1 d . . . H18A H 0.6178 0.0379 0.7458 0.102(9) Uiso 1 1 calc R . . H18B H 0.5772 0.1911 0.7579 0.102(9) Uiso 1 1 calc R . . C19 C 0.5744(2) 0.1413(8) 0.6837(2) 0.0588(15) Uani 1 1 d . . . H19A H 0.5867 0.2573 0.6793 0.102(9) Uiso 1 1 calc R . . H19B H 0.5977 0.0674 0.6649 0.102(9) Uiso 1 1 calc R . . O100 O 0.1975(3) -0.4335(6) 0.6894(2) 0.0459(14) Uani 0.60 1 d P . . C100 C 0.1893(4) -0.5935(10) 0.6648(4) 0.052(2) Uani 0.60 1 d P . . H10A H 0.1601 -0.5832 0.6375 0.088(11) Uiso 0.60 1 calc PR . . H10B H 0.2255 -0.6311 0.6527 0.088(11) Uiso 0.60 1 calc PR . . C101 C 0.1706(5) -0.7112(11) 0.6996(5) 0.080(4) Uani 0.60 1 d P . . H10C H 0.1329 -0.7584 0.6884 0.088(11) Uiso 0.60 1 calc PR . . H10D H 0.1984 -0.8029 0.7045 0.088(11) Uiso 0.60 1 calc PR . . C102 C 0.1665(6) -0.6220(15) 0.7433(6) 0.106(5) Uani 0.60 1 d P . . H10E H 0.1829 -0.6881 0.7708 0.088(11) Uiso 0.60 1 calc PR . . H10F H 0.1261 -0.5972 0.7481 0.088(11) Uiso 0.60 1 calc PR . . C103 C 0.2003(4) -0.4614(10) 0.7390(3) 0.053(2) Uani 0.60 1 d P . . H10G H 0.1825 -0.3689 0.7556 0.088(11) Uiso 0.60 1 calc PR . . H10H H 0.2403 -0.4747 0.7524 0.088(11) Uiso 0.60 1 calc PR . . O20 O 0.2500 0.3587(11) 0.5000 0.095(6) Uani 0.50 2 d SP . 1 C20 C 0.2552(6) 0.4736(18) 0.4580(5) 0.072(4) Uiso 0.50 1 d P A 1 H20A H 0.2321 0.4331 0.4293 0.088(11) Uiso 0.50 1 calc PR A 1 H20B H 0.2955 0.4854 0.4506 0.088(11) Uiso 0.50 1 calc PR A 1 C21 C 0.2303(8) 0.647(2) 0.4766(7) 0.088(4) Uiso 0.50 1 d P . 1 H21A H 0.2375 0.7415 0.4555 0.088(11) Uiso 0.50 1 calc PR . 1 H21B H 0.1892 0.6407 0.4821 0.088(11) Uiso 0.50 1 calc PR . 1 O20X O 0.2500 0.654(9) 0.5000 0.14(2) Uiso 0.20 2 d SP . 2 C20X C 0.2645(10) 0.386(3) 0.4745(8) 0.024(5) Uiso 0.20 1 d P . 2 H20C H 0.2982 0.3116 0.4759 0.088(11) Uiso 0.20 1 calc PR . 2 H20D H 0.2367 0.3486 0.4484 0.088(11) Uiso 0.20 1 calc PR . 2 C21X C 0.2827(8) 0.569(2) 0.4665(7) 0.023(4) Uiso 0.20 1 d P B 2 H21C H 0.3243 0.5848 0.4741 0.088(11) Uiso 0.20 1 calc PR B 2 H21D H 0.2721 0.6056 0.4334 0.088(11) Uiso 0.20 1 calc PR B 2 H1 H 0.208(2) -0.217(6) 0.6584(19) 0.028(14) Uiso 1 1 d . . . H2 H 0.334(2) 0.202(7) 0.5731(19) 0.049(14) Uiso 1 1 d . . . H3 H 0.230(2) 0.114(6) 0.5952(17) 0.041(13) Uiso 1 1 d . . . H5 H 0.302(2) -0.330(7) 0.6537(19) 0.054(15) Uiso 1 1 d . . . H6 H 0.401(3) -0.251(7) 0.643(3) 0.07(2) Uiso 1 1 d . . . H7 H 0.455(2) -0.198(6) 0.5661(17) 0.036(13) Uiso 1 1 d . . . H9 H 0.537(2) -0.282(6) 0.5405(19) 0.043(14) Uiso 1 1 d . . . H10 H 0.639(3) -0.163(8) 0.522(2) 0.061(17) Uiso 1 1 d . . . H11 H 0.669(2) 0.115(7) 0.528(2) 0.064(16) Uiso 1 1 d . . . H12 H 0.598(3) 0.297(9) 0.559(3) 0.09(2) Uiso 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 0.0437(3) 0.0272(2) 0.0368(2) 0.00434(15) -0.00636(17) -0.00286(16) O1 0.049(2) 0.061(3) 0.081(3) 0.000(2) 0.010(2) -0.005(2) O13 0.087(3) 0.041(2) 0.064(3) 0.0025(17) -0.017(2) -0.022(2) O14 0.091(3) 0.0351(19) 0.047(2) 0.0097(15) -0.0148(19) 0.0065(18) O15 0.063(2) 0.0389(19) 0.048(2) -0.0033(15) -0.0019(18) 0.0042(17) O16 0.0411(18) 0.046(2) 0.048(2) 0.0163(15) -0.0044(15) -0.0036(14) N1 0.039(2) 0.033(2) 0.035(2) 0.0040(15) -0.0021(16) 0.0013(16) N2 0.045(2) 0.038(2) 0.034(2) 0.0045(15) -0.0025(17) -0.0060(17) C1 0.046(3) 0.030(2) 0.041(3) -0.0018(18) -0.004(2) 0.0000(19) C2 0.039(3) 0.032(2) 0.053(3) -0.005(2) -0.006(2) 0.0002(19) C3 0.045(3) 0.042(3) 0.053(3) -0.010(2) -0.005(2) 0.001(2) C4 0.039(3) 0.050(3) 0.064(4) -0.012(2) 0.006(2) -0.009(2) C5 0.049(3) 0.038(3) 0.054(3) -0.001(2) 0.002(2) -0.005(2) C6 0.047(3) 0.028(2) 0.055(3) -0.003(2) 0.001(2) -0.001(2) C7 0.043(3) 0.027(2) 0.036(2) 0.0022(17) -0.0041(19) 0.0022(19) C8 0.049(3) 0.042(3) 0.030(2) 0.0029(18) -0.003(2) 0.003(2) C9 0.056(3) 0.054(3) 0.030(2) 0.006(2) -0.001(2) 0.014(3) C10 0.051(3) 0.072(4) 0.035(3) 0.003(2) 0.004(2) 0.008(3) C11 0.043(3) 0.092(5) 0.036(3) 0.004(3) 0.003(2) 0.000(3) C12 0.053(3) 0.059(3) 0.039(3) 0.009(2) -0.004(2) -0.011(3) C13 0.054(3) 0.043(3) 0.044(3) 0.012(2) -0.011(2) -0.009(2) C14 0.055(3) 0.027(2) 0.042(3) 0.0013(18) -0.003(2) -0.003(2) C15 0.050(3) 0.023(2) 0.043(3) 0.0010(17) -0.008(2) -0.0029(19) C16 0.063(3) 0.049(3) 0.045(3) 0.009(2) 0.001(3) -0.004(2) C17 0.054(4) 0.121(6) 0.071(4) 0.044(4) -0.004(3) -0.012(4) C18 0.057(3) 0.064(4) 0.047(3) 0.006(3) -0.006(3) -0.002(3) C19 0.042(3) 0.077(4) 0.057(3) 0.021(3) -0.004(2) -0.004(3) O100 0.070(4) 0.020(3) 0.052(3) -0.003(2) 0.033(3) -0.015(2) C100 0.047(5) 0.033(4) 0.075(6) -0.018(4) 0.004(4) -0.001(4) C101 0.073(7) 0.027(5) 0.134(12) 0.017(6) -0.033(7) -0.006(5) C102 0.127(11) 0.071(8) 0.134(12) 0.048(8) 0.097(10) -0.002(7) C103 0.074(6) 0.026(4) 0.059(6) 0.005(4) 0.001(5) 0.005(4) O20 0.178(15) 0.002(5) 0.094(12) 0.000 -0.067(11) 0.000 _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 C14 1.922(5) . ? Mo1 C15 1.942(5) . ? Mo1 C13 1.943(5) . ? Mo1 N1 2.254(4) . ? Mo1 N2 2.275(4) . ? Mo1 O16 2.289(3) . ? O1 C4 1.378(6) . ? O1 H1 0.76(5) . ? O13 C13 1.178(6) . ? O14 C14 1.176(5) . ? O15 C15 1.169(6) . ? O16 C16 1.430(6) . ? O16 C19 1.455(6) . ? N1 C7 1.272(6) . ? N1 C1 1.431(6) . ? N2 C12 1.344(6) . ? N2 C8 1.367(6) . ? C1 C6 1.400(7) . ? C1 C2 1.423(6) . ? C2 C3 1.376(7) . ? C2 H2 1.12(5) . ? C3 C4 1.382(8) . ? C3 H3 1.06(5) . ? C4 C5 1.394(7) . ? C5 C6 1.362(7) . ? C5 H5 0.96(6) . ? C6 H6 1.14(7) . ? C7 C8 1.458(7) . ? C7 H7 0.89(5) . ? C8 C9 1.385(7) . ? C9 C10 1.368(8) . ? C9 H9 1.10(5) . ? C10 C11 1.360(9) . ? C10 H10 0.88(6) . ? C11 C12 1.396(8) . ? C11 H11 1.12(6) . ? C12 H12 1.00(7) . ? C16 C17 1.455(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.500(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.520(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? O100 C103 1.380(10) . ? O100 C100 1.440(9) . ? C100 C101 1.428(15) . ? C100 H10A 0.9700 . ? C100 H10B 0.9700 . ? C101 C102 1.405(18) . ? C101 H10C 0.9700 . ? C101 H10D 0.9700 . ? C102 C103 1.498(14) . ? C102 H10E 0.9700 . ? C102 H10F 0.9700 . ? C103 H10G 0.9700 . ? C103 H10H 0.9700 . ? O20 C20 1.484(15) 2_556 ? O20 C20 1.484(15) . ? C20 C21 1.58(2) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C21 1.52(4) 2_556 ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? O20X C21X 1.41(4) 2_556 ? O20X C21X 1.41(4) . ? C20X C21X 1.53(3) . ? C20X C20X 1.60(4) 2_556 ? C20X H20C 0.9700 . ? C20X H20D 0.9700 . ? C21X H21C 0.9700 . ? C21X H21D 0.9700 . ? 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 C14 Mo1 C15 85.7(2) . . ? C14 Mo1 C13 84.69(19) . . ? C15 Mo1 C13 86.9(2) . . ? C14 Mo1 N1 101.91(16) . . ? C15 Mo1 N1 96.85(16) . . ? C13 Mo1 N1 172.58(17) . . ? C14 Mo1 N2 99.27(18) . . ? C15 Mo1 N2 168.84(16) . . ? C13 Mo1 N2 103.40(19) . . ? N1 Mo1 N2 72.42(13) . . ? C14 Mo1 O16 175.70(17) . . ? C15 Mo1 O16 97.75(16) . . ? C13 Mo1 O16 92.95(16) . . ? N1 Mo1 O16 80.24(12) . . ? N2 Mo1 O16 77.74(13) . . ? C4 O1 H1 103(4) . . ? C16 O16 C19 109.6(4) . . ? C16 O16 Mo1 127.2(3) . . ? C19 O16 Mo1 122.2(3) . . ? C7 N1 C1 118.6(4) . . ? C7 N1 Mo1 116.5(3) . . ? C1 N1 Mo1 124.3(3) . . ? C12 N2 C8 116.5(4) . . ? C12 N2 Mo1 128.3(4) . . ? C8 N2 Mo1 114.7(3) . . ? C6 C1 C2 118.4(5) . . ? C6 C1 N1 122.8(4) . . ? C2 C1 N1 118.7(4) . . ? C3 C2 C1 120.4(5) . . ? C3 C2 H2 126(3) . . ? C1 C2 H2 114(3) . . ? C2 C3 C4 119.6(5) . . ? C2 C3 H3 123(3) . . ? C4 C3 H3 117(3) . . ? O1 C4 C3 115.8(5) . . ? O1 C4 C5 123.6(5) . . ? C3 C4 C5 120.6(5) . . ? C6 C5 C4 120.4(5) . . ? C6 C5 H5 116(3) . . ? C4 C5 H5 123(3) . . ? C5 C6 C1 120.6(5) . . ? C5 C6 H6 120(3) . . ? C1 C6 H6 117(3) . . ? N1 C7 C8 119.9(4) . . ? N1 C7 H7 131(3) . . ? C8 C7 H7 109(3) . . ? N2 C8 C9 122.7(5) . . ? N2 C8 C7 115.0(4) . . ? C9 C8 C7 122.3(5) . . ? C10 C9 C8 119.1(5) . . ? C10 C9 H9 131(3) . . ? C8 C9 H9 110(3) . . ? C11 C10 C9 119.6(6) . . ? C11 C10 H10 113(4) . . ? C9 C10 H10 127(4) . . ? C10 C11 C12 119.1(6) . . ? C10 C11 H11 121(3) . . ? C12 C11 H11 119(3) . . ? N2 C12 C11 122.9(5) . . ? N2 C12 H12 122(4) . . ? C11 C12 H12 115(4) . . ? O13 C13 Mo1 175.6(5) . . ? O14 C14 Mo1 176.4(4) . . ? O15 C15 Mo1 178.2(4) . . ? O16 C16 C17 107.7(5) . . ? O16 C16 H16A 110.2 . . ? C17 C16 H16A 110.2 . . ? O16 C16 H16B 110.2 . . ? C17 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? C16 C17 C18 106.7(5) . . ? C16 C17 H17A 110.4 . . ? C18 C17 H17A 110.4 . . ? C16 C17 H17B 110.4 . . ? C18 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? C17 C18 C19 102.9(5) . . ? C17 C18 H18A 111.2 . . ? C19 C18 H18A 111.2 . . ? C17 C18 H18B 111.2 . . ? C19 C18 H18B 111.2 . . ? H18A C18 H18B 109.1 . . ? O16 C19 C18 105.0(4) . . ? O16 C19 H19A 110.8 . . ? C18 C19 H19A 110.8 . . ? O16 C19 H19B 110.8 . . ? C18 C19 H19B 110.8 . . ? H19A C19 H19B 108.8 . . ? C103 O100 C100 108.6(6) . . ? C101 C100 O100 106.9(8) . . ? C101 C100 H10A 110.3 . . ? O100 C100 H10A 110.3 . . ? C101 C100 H10B 110.3 . . ? O100 C100 H10B 110.3 . . ? H10A C100 H10B 108.6 . . ? C102 C101 C100 107.1(8) . . ? C102 C101 H10C 110.3 . . ? C100 C101 H10C 110.3 . . ? C102 C101 H10D 110.3 . . ? C100 C101 H10D 110.3 . . ? H10C C101 H10D 108.6 . . ? C101 C102 C103 106.6(8) . . ? C101 C102 H10E 110.4 . . ? C103 C102 H10E 110.4 . . ? C101 C102 H10F 110.4 . . ? C103 C102 H10F 110.4 . . ? H10E C102 H10F 108.6 . . ? O100 C103 C102 103.5(9) . . ? O100 C103 H10G 111.1 . . ? C102 C103 H10G 111.1 . . ? O100 C103 H10H 111.1 . . ? C102 C103 H10H 111.1 . . ? H10G C103 H10H 109.0 . . ? C20 O20 C20 104.5(12) 2_556 . ? O20 C20 C21 102.9(11) . . ? O20 C20 H20A 111.2 . . ? C21 C20 H20A 111.2 . . ? O20 C20 H20B 111.2 . . ? C21 C20 H20B 111.2 . . ? H20A C20 H20B 109.1 . . ? C21 C21 C20 93.9(11) 2_556 . ? C21 C21 H21A 112.9 2_556 . ? C20 C21 H21A 112.9 . . ? C21 C21 H21B 112.9 2_556 . ? C20 C21 H21B 112.9 . . ? H21A C21 H21B 110.4 . . ? C21X O20X C21X 123(5) 2_556 . ? C21X C20X C20X 105.4(11) . 2_556 ? C21X C20X H20C 110.7 . . ? C20X C20X H20C 110.7 2_556 . ? C21X C20X H20D 110.7 . . ? C20X C20X H20D 110.7 2_556 . ? H20C C20X H20D 108.8 . . ? O20X C21X C20X 101(3) . . ? O20X C21X H21C 111.6 . . ? C20X C21X H21C 111.6 . . ? O20X C21X H21D 111.6 . . ? C20X C21X H21D 111.6 . . ? H21C C21X H21D 109.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 Mo1 O16 C16 -175(2) . . . . ? C15 Mo1 O16 C16 40.7(4) . . . . ? C13 Mo1 O16 C16 128.0(4) . . . . ? N1 Mo1 O16 C16 -54.9(4) . . . . ? N2 Mo1 O16 C16 -128.9(4) . . . . ? C14 Mo1 O16 C19 17(2) . . . . ? C15 Mo1 O16 C19 -126.9(4) . . . . ? C13 Mo1 O16 C19 -39.6(4) . . . . ? N1 Mo1 O16 C19 137.5(4) . . . . ? N2 Mo1 O16 C19 63.5(4) . . . . ? C14 Mo1 N1 C7 105.5(4) . . . . ? C15 Mo1 N1 C7 -167.4(3) . . . . ? C13 Mo1 N1 C7 -47.1(15) . . . . ? N2 Mo1 N1 C7 9.5(3) . . . . ? O16 Mo1 N1 C7 -70.7(3) . . . . ? C14 Mo1 N1 C1 -83.8(4) . . . . ? C15 Mo1 N1 C1 3.3(4) . . . . ? C13 Mo1 N1 C1 123.6(14) . . . . ? N2 Mo1 N1 C1 -179.8(4) . . . . ? O16 Mo1 N1 C1 100.0(3) . . . . ? C14 Mo1 N2 C12 78.0(4) . . . . ? C15 Mo1 N2 C12 -166.0(8) . . . . ? C13 Mo1 N2 C12 -8.7(4) . . . . ? N1 Mo1 N2 C12 177.7(4) . . . . ? O16 Mo1 N2 C12 -98.8(4) . . . . ? C14 Mo1 N2 C8 -109.8(3) . . . . ? C15 Mo1 N2 C8 6.1(10) . . . . ? C13 Mo1 N2 C8 163.5(3) . . . . ? N1 Mo1 N2 C8 -10.2(3) . . . . ? O16 Mo1 N2 C8 73.3(3) . . . . ? C7 N1 C1 C6 41.5(6) . . . . ? Mo1 N1 C1 C6 -129.0(4) . . . . ? C7 N1 C1 C2 -142.5(4) . . . . ? Mo1 N1 C1 C2 47.0(5) . . . . ? C6 C1 C2 C3 -1.0(7) . . . . ? N1 C1 C2 C3 -177.2(4) . . . . ? C1 C2 C3 C4 2.3(7) . . . . ? C2 C3 C4 O1 177.4(5) . . . . ? C2 C3 C4 C5 -2.3(8) . . . . ? O1 C4 C5 C6 -178.6(5) . . . . ? C3 C4 C5 C6 1.0(8) . . . . ? C4 C5 C6 C1 0.3(8) . . . . ? C2 C1 C6 C5 -0.3(7) . . . . ? N1 C1 C6 C5 175.7(5) . . . . ? C1 N1 C7 C8 -178.9(4) . . . . ? Mo1 N1 C7 C8 -7.7(5) . . . . ? C12 N2 C8 C9 0.9(6) . . . . ? Mo1 N2 C8 C9 -172.2(3) . . . . ? C12 N2 C8 C7 -176.8(4) . . . . ? Mo1 N2 C8 C7 10.1(5) . . . . ? N1 C7 C8 N2 -1.8(6) . . . . ? N1 C7 C8 C9 -179.5(4) . . . . ? N2 C8 C9 C10 0.4(7) . . . . ? C7 C8 C9 C10 178.0(4) . . . . ? C8 C9 C10 C11 -1.1(7) . . . . ? C9 C10 C11 C12 0.4(8) . . . . ? C8 N2 C12 C11 -1.7(7) . . . . ? Mo1 N2 C12 C11 170.4(4) . . . . ? C10 C11 C12 N2 1.1(8) . . . . ? C14 Mo1 C13 O13 59(6) . . . . ? C15 Mo1 C13 O13 -27(6) . . . . ? N1 Mo1 C13 O13 -148(5) . . . . ? N2 Mo1 C13 O13 157(6) . . . . ? O16 Mo1 C13 O13 -125(6) . . . . ? C15 Mo1 C14 O14 59(7) . . . . ? C13 Mo1 C14 O14 -28(7) . . . . ? N1 Mo1 C14 O14 156(7) . . . . ? N2 Mo1 C14 O14 -131(7) . . . . ? O16 Mo1 C14 O14 -85(8) . . . . ? C14 Mo1 C15 O15 66(13) . . . . ? C13 Mo1 C15 O15 151(13) . . . . ? N1 Mo1 C15 O15 -35(13) . . . . ? N2 Mo1 C15 O15 -51(14) . . . . ? O16 Mo1 C15 O15 -116(13) . . . . ? C19 O16 C16 C17 0.7(7) . . . . ? Mo1 O16 C16 C17 -168.1(4) . . . . ? O16 C16 C17 C18 17.0(8) . . . . ? C16 C17 C18 C19 -27.0(7) . . . . ? C16 O16 C19 C18 -17.8(6) . . . . ? Mo1 O16 C19 C18 151.8(3) . . . . ? C17 C18 C19 O16 27.0(7) . . . . ? C103 O100 C100 C101 16.3(10) . . . . ? O100 C100 C101 C102 1.3(13) . . . . ? C100 C101 C102 C103 -16.9(14) . . . . ? C100 O100 C103 C102 -25.7(10) . . . . ? C101 C102 C103 O100 26.5(13) . . . . ? C20 O20 C20 C21 -19.3(8) 2_556 . . . ? O20 C20 C21 C21 52.0(14) . . . 2_556 ? C21X O20X C21X C20X 6.8(10) 2_556 . . . ? C20X C20X C21X O20X -17(2) 2_556 . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.328 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.130 #===END # 1. SUBMISSION DETAILS #============================================================================== data_ka269 _database_code_CSD 168309 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H25 Mo N2 O4.50 P' _chemical_formula_weight 672.48 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' 'P' 'P' 0.1023 0.0942 '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 monoklin _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.7180(17) _cell_length_b 16.681(3) _cell_length_c 21.761(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.32(3) _cell_angle_gamma 90.00 _cell_volume 3150.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.510 _exptl_absorpt_correction_type 'experimentell' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _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 'NONIUS KAPPA CCD' _diffrn_measurement_method 'O-Scan ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20837 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 32.05 _reflns_number_total 10893 _reflns_number_gt 7255 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0593P)^2^+0.1537P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10893 _refine_ls_number_parameters 492 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1248 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.340 _refine_ls_shift/su_mean 0.019 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.20247(2) 0.889039(13) 0.100763(9) 0.01980(7) Uani 1 1 d . . . P1 P 0.28515(7) 0.87182(4) 0.21468(3) 0.02178(14) Uani 1 1 d . . . O1 O 0.6205(2) 0.54726(14) 0.02373(12) 0.0388(5) Uani 1 1 d . . . O13 O -0.1116(2) 0.95593(13) 0.13596(10) 0.0383(5) Uani 1 1 d . . . O14 O 0.0461(3) 0.89585(15) -0.03426(10) 0.0508(6) Uani 1 1 d . . . O15 O 0.0484(2) 0.72052(12) 0.10034(9) 0.0377(5) Uani 1 1 d . . . N1 N 0.4415(2) 0.85926(13) 0.07426(9) 0.0237(4) Uani 1 1 d . . . N2 N 0.3354(2) 1.00454(13) 0.09893(10) 0.0251(5) Uani 1 1 d . . . C1 C 0.4933(3) 0.78108(15) 0.05928(12) 0.0240(5) Uani 1 1 d . . . C2 C 0.3900(3) 0.72880(16) 0.02901(12) 0.0254(5) Uani 1 1 d . . . C3 C 0.4313(3) 0.65094(17) 0.01634(12) 0.0284(6) Uani 1 1 d . . . C4 C 0.5794(3) 0.62501(16) 0.03514(13) 0.0288(6) Uani 1 1 d . . . C5 C 0.6853(3) 0.67670(18) 0.06517(14) 0.0318(6) Uani 1 1 d . . . C6 C 0.6433(3) 0.75487(18) 0.07717(13) 0.0291(6) Uani 1 1 d . . . C7 C 0.5369(3) 0.91910(17) 0.07273(12) 0.0263(5) Uani 1 1 d . . . C8 C 0.4850(3) 0.99906(16) 0.08656(12) 0.0255(5) Uani 1 1 d . . . C9 C 0.5817(3) 1.06504(17) 0.08571(13) 0.0315(6) Uani 1 1 d . . . C10 C 0.5239(4) 1.14031(19) 0.09746(14) 0.0357(6) Uani 1 1 d . . . C11 C 0.3715(4) 1.14609(19) 0.10941(15) 0.0368(7) Uani 1 1 d . . . C12 C 0.2826(3) 1.07832(17) 0.10998(13) 0.0300(6) Uani 1 1 d . . . C13 C 0.0073(3) 0.93204(16) 0.12346(12) 0.0270(5) Uani 1 1 d . . . C14 C 0.1098(3) 0.89660(17) 0.01441(13) 0.0297(6) Uani 1 1 d . . . C15 C 0.1079(3) 0.78356(16) 0.10081(12) 0.0256(5) Uani 1 1 d . . . C20 C 0.1278(3) 0.86672(16) 0.26543(12) 0.0241(5) Uani 1 1 d . . . C21 C 0.0029(3) 0.81804(17) 0.24760(13) 0.0277(6) Uani 1 1 d . . . C22 C -0.1150(3) 0.80622(18) 0.28577(14) 0.0327(6) Uani 1 1 d . . . C23 C -0.1094(3) 0.8445(2) 0.34158(14) 0.0372(7) Uani 1 1 d . . . C24 C 0.0138(4) 0.8945(2) 0.36038(15) 0.0425(8) Uani 1 1 d . . . C25 C 0.1323(3) 0.9048(2) 0.32228(14) 0.0355(7) Uani 1 1 d . . . C30 C 0.4070(3) 0.95354(16) 0.24598(11) 0.0239(5) Uani 1 1 d . . . C31 C 0.5674(3) 0.94562(18) 0.25353(14) 0.0318(6) Uani 1 1 d . . . C32 C 0.6592(3) 1.0107(2) 0.27194(16) 0.0426(8) Uani 1 1 d . . . C33 C 0.5941(4) 1.0843(2) 0.28318(16) 0.0419(7) Uani 1 1 d . . . C34 C 0.4354(4) 1.0931(2) 0.27466(15) 0.0395(7) Uani 1 1 d . . . C35 C 0.3441(3) 1.02814(18) 0.25537(14) 0.0324(6) Uani 1 1 d . . . C40 C 0.3923(3) 0.78172(16) 0.24229(12) 0.0247(5) Uani 1 1 d . . . C41 C 0.4191(3) 0.71929(17) 0.20225(13) 0.0290(6) Uani 1 1 d . . . C42 C 0.4970(3) 0.65085(18) 0.22443(15) 0.0358(7) Uani 1 1 d . . . C43 C 0.5473(3) 0.64323(19) 0.28626(15) 0.0378(7) Uani 1 1 d . . . C44 C 0.5210(3) 0.70511(19) 0.32686(15) 0.0361(7) Uani 1 1 d . . . C45 C 0.4437(3) 0.77377(18) 0.30531(13) 0.0306(6) Uani 1 1 d . . . H1 H 0.557(9) 0.524(5) 0.020(4) 0.08(2) Uiso 0.50 1 d P A 1 H1X H 0.7414 0.5242 0.0138 0.08(2) Uiso 0.50 1 d P B 2 H2 H 0.294(3) 0.7496(18) 0.0171(13) 0.037(8) Uiso 1 1 d . . . H3 H 0.350(3) 0.6117(16) -0.0059(14) 0.031(8) Uiso 1 1 d . . . H5 H 0.779(3) 0.6612(19) 0.0758(13) 0.040(9) Uiso 1 1 d . . . H6 H 0.708(3) 0.787(2) 0.1019(13) 0.040(9) Uiso 1 1 d . . . H7 H 0.644(3) 0.9134(17) 0.0613(13) 0.032(8) Uiso 1 1 d . . . H9 H 0.687(3) 1.0585(18) 0.0741(13) 0.036(8) Uiso 1 1 d . . . H10 H 0.586(3) 1.1903(17) 0.1046(12) 0.028(7) Uiso 1 1 d . . . H11 H 0.334(3) 1.1928(19) 0.1147(14) 0.037(9) Uiso 1 1 d . . . H12 H 0.178(3) 1.0793(19) 0.1128(13) 0.036(8) Uiso 1 1 d . . . H31 H 0.607(4) 0.8921(18) 0.2509(14) 0.036(9) Uiso 1 1 d . . . H32 H 0.787(4) 1.002(2) 0.2763(16) 0.063(11) Uiso 1 1 d . . . H33 H 0.656(3) 1.1268(17) 0.2962(13) 0.025(7) Uiso 1 1 d . . . H34 H 0.389(4) 1.145(2) 0.2792(14) 0.047(9) Uiso 1 1 d . . . H35 H 0.237(4) 1.033(2) 0.2490(15) 0.053(10) Uiso 1 1 d . . . H21 H -0.003(3) 0.7911(16) 0.2122(13) 0.021(7) Uiso 1 1 d . . . H22 H -0.204(3) 0.7696(19) 0.2717(13) 0.039(8) Uiso 1 1 d . . . H23 H -0.179(3) 0.8366(19) 0.3631(14) 0.039(9) Uiso 1 1 d . . . H24 H 0.028(4) 0.917(2) 0.4022(18) 0.066(12) Uiso 1 1 d . . . H25 H 0.209(3) 0.9400(19) 0.3267(14) 0.040(9) Uiso 1 1 d . . . H41 H 0.3813 0.7371 0.1548 0.077(12) Uiso 1 1 d . . . H42 H 0.517(4) 0.6066(19) 0.1897(15) 0.047(10) Uiso 1 1 d . . . H43 H 0.604(4) 0.5927(19) 0.3024(14) 0.044(9) Uiso 1 1 d . . . H44 H 0.544(3) 0.7021(18) 0.3725(14) 0.038(8) Uiso 1 1 d . . . H45 H 0.427(3) 0.8206(18) 0.3368(14) 0.038(8) Uiso 1 1 d . . . O100 O 0.9061(5) 0.5085(3) 0.0232(2) 0.0608(14) Uani 0.50 1 d P . . C100 C 0.9867(9) 0.6269(5) -0.0396(4) 0.0427(18) Uiso 0.50 1 d P . . C101 C 1.0440(18) 0.5580(10) 0.0089(8) 0.148(5) Uiso 0.50 1 d P . . C102 C 0.9736(9) 0.4519(5) 0.0709(4) 0.060(2) Uiso 0.50 1 d P . . C103 C 1.0237(17) 0.4024(9) 0.0455(7) 0.105(5) 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 0.01688(9) 0.02158(12) 0.02084(11) -0.00016(9) 0.00121(7) 0.00052(8) P1 0.0183(3) 0.0240(4) 0.0231(3) 0.0008(3) 0.0021(2) 0.0004(2) O1 0.0289(10) 0.0288(12) 0.0588(14) -0.0100(10) 0.0049(10) 0.0034(8) O13 0.0233(9) 0.0414(13) 0.0507(13) 0.0004(10) 0.0065(8) 0.0079(8) O14 0.0490(13) 0.0732(18) 0.0281(12) 0.0005(11) -0.0071(9) 0.0006(11) O15 0.0360(10) 0.0344(12) 0.0428(12) -0.0025(10) 0.0046(9) -0.0088(9) N1 0.0221(10) 0.0256(12) 0.0234(11) -0.0025(9) 0.0024(8) -0.0001(8) N2 0.0233(10) 0.0255(12) 0.0265(11) 0.0004(9) 0.0023(8) -0.0007(8) C1 0.0235(11) 0.0228(13) 0.0262(13) -0.0003(10) 0.0054(9) 0.0012(9) C2 0.0192(11) 0.0278(14) 0.0294(14) -0.0028(11) 0.0033(9) 0.0022(9) C3 0.0224(12) 0.0311(16) 0.0312(14) -0.0057(12) 0.0004(10) -0.0025(10) C4 0.0275(12) 0.0234(15) 0.0359(15) -0.0048(11) 0.0055(11) 0.0030(10) C5 0.0223(12) 0.0308(16) 0.0421(17) -0.0059(13) 0.0017(11) 0.0025(11) C6 0.0217(11) 0.0298(15) 0.0356(15) -0.0039(12) 0.0022(10) -0.0029(10) C7 0.0210(11) 0.0287(14) 0.0294(14) -0.0015(11) 0.0033(10) -0.0018(10) C8 0.0228(11) 0.0288(15) 0.0249(13) 0.0024(11) 0.0027(9) 0.0000(10) C9 0.0308(13) 0.0297(16) 0.0340(15) -0.0013(12) 0.0027(11) -0.0055(11) C10 0.0423(16) 0.0283(16) 0.0364(16) 0.0014(13) 0.0026(12) -0.0095(13) C11 0.0443(16) 0.0242(16) 0.0423(18) 0.0013(14) 0.0061(13) 0.0038(13) C12 0.0305(13) 0.0255(15) 0.0339(15) 0.0008(12) 0.0031(11) 0.0001(11) C13 0.0263(12) 0.0251(14) 0.0294(14) -0.0007(11) 0.0010(10) 0.0010(10) C14 0.0302(13) 0.0321(16) 0.0267(14) 0.0020(12) 0.0030(10) 0.0003(11) C15 0.0216(11) 0.0283(15) 0.0267(13) -0.0042(11) 0.0015(9) -0.0016(10) C20 0.0202(11) 0.0271(14) 0.0254(13) 0.0039(11) 0.0049(9) 0.0017(9) C21 0.0252(12) 0.0290(15) 0.0297(14) 0.0009(12) 0.0066(10) 0.0014(10) C22 0.0263(12) 0.0302(16) 0.0428(17) 0.0066(13) 0.0093(11) 0.0015(11) C23 0.0308(14) 0.0442(19) 0.0391(17) 0.0090(14) 0.0169(12) 0.0024(12) C24 0.0404(16) 0.056(2) 0.0329(17) -0.0047(15) 0.0140(13) -0.0008(14) C25 0.0308(14) 0.0454(19) 0.0311(15) -0.0047(13) 0.0067(11) -0.0052(13) C30 0.0243(11) 0.0273(14) 0.0200(12) 0.0006(10) 0.0013(9) -0.0014(10) C31 0.0242(12) 0.0294(16) 0.0417(17) 0.0044(13) 0.0025(11) -0.0023(11) C32 0.0292(14) 0.0374(18) 0.060(2) 0.0085(16) -0.0020(13) -0.0085(12) C33 0.0409(16) 0.0349(18) 0.0481(19) 0.0047(15) -0.0058(14) -0.0151(14) C34 0.0429(16) 0.0304(17) 0.0450(19) -0.0095(14) 0.0035(13) -0.0028(13) C35 0.0272(13) 0.0329(16) 0.0367(16) -0.0038(13) 0.0013(11) 0.0020(11) C40 0.0191(10) 0.0247(14) 0.0305(14) 0.0057(11) 0.0038(9) 0.0001(9) C41 0.0253(12) 0.0297(15) 0.0326(15) 0.0042(12) 0.0063(10) 0.0037(10) C42 0.0330(14) 0.0298(17) 0.0454(18) 0.0011(14) 0.0088(12) 0.0045(12) C43 0.0293(14) 0.0332(17) 0.0514(19) 0.0179(15) 0.0065(12) 0.0050(12) C44 0.0314(14) 0.0418(18) 0.0347(16) 0.0157(14) 0.0014(11) 0.0011(12) C45 0.0295(13) 0.0327(16) 0.0292(14) 0.0051(12) 0.0007(10) 0.0001(11) O100 0.039(3) 0.080(4) 0.065(3) 0.019(3) 0.019(2) 0.022(2) _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 C15 1.943(3) . ? Mo1 C13 1.952(2) . ? Mo1 C14 1.979(3) . ? Mo1 N2 2.250(2) . ? Mo1 N1 2.268(2) . ? Mo1 P1 2.5328(9) . ? P1 C30 1.821(3) . ? P1 C40 1.841(3) . ? P1 C20 1.841(2) . ? O1 C4 1.374(3) . ? O1 H1 0.67(7) . ? O1 H1X 1.161(2) . ? O13 C13 1.165(3) . ? O14 C14 1.149(3) . ? O15 C15 1.172(3) . ? N1 C7 1.301(3) . ? N1 C1 1.428(3) . ? N2 C12 1.343(3) . ? N2 C8 1.360(3) . ? C1 C2 1.377(3) . ? C1 C6 1.399(3) . ? C2 C3 1.382(4) . ? C2 H2 0.92(3) . ? C3 C4 1.387(4) . ? C3 H3 1.05(3) . ? C4 C5 1.382(4) . ? C5 C6 1.386(4) . ? C5 H5 0.87(3) . ? C6 H6 0.91(3) . ? C7 C8 1.449(4) . ? C7 H7 1.00(3) . ? C8 C9 1.387(4) . ? C9 C10 1.386(4) . ? C9 H9 0.98(3) . ? C10 C11 1.381(4) . ? C10 H10 1.00(3) . ? C11 C12 1.371(4) . ? C11 H11 0.86(3) . ? C12 H12 0.92(3) . ? C20 C21 1.384(4) . ? C20 C25 1.388(4) . ? C21 C22 1.395(3) . ? C21 H21 0.89(3) . ? C22 C23 1.369(4) . ? C22 H22 1.02(3) . ? C23 C24 1.392(5) . ? C23 H23 0.81(3) . ? C24 C25 1.394(4) . ? C24 H24 0.98(4) . ? C25 H25 0.89(3) . ? C30 C35 1.383(4) . ? C30 C31 1.399(3) . ? C31 C32 1.386(4) . ? C31 H31 0.96(3) . ? C32 C33 1.384(5) . ? C32 H32 1.12(4) . ? C33 C34 1.386(4) . ? C33 H33 0.92(3) . ? C34 C35 1.386(4) . ? C34 H34 0.97(3) . ? C35 H35 0.94(3) . ? C40 C41 1.391(4) . ? C40 C45 1.409(4) . ? C41 C42 1.392(4) . ? C41 H41 1.095(3) . ? C42 C43 1.382(4) . ? C42 H42 1.08(3) . ? C43 C44 1.392(5) . ? C43 H43 1.02(3) . ? C44 C45 1.388(4) . ? C44 H44 0.99(3) . ? C45 H45 1.06(3) . ? O100 C101 1.402(16) 3_765 ? O100 C102 1.483(9) . ? O100 C101 1.515(15) . ? O100 H1X 1.455(4) . ? C100 C103 0.513(17) 3_765 ? C100 C102 1.536(12) 3_765 ? C100 C101 1.608(19) . ? C101 O100 1.402(16) 3_765 ? C101 C103 1.434(19) 3_765 ? C101 C102 1.737(18) 3_765 ? C102 C103 1.105(14) . ? C102 C100 1.536(12) 3_765 ? C102 C101 1.737(18) 3_765 ? C103 C100 0.513(17) 3_765 ? C103 C101 1.434(19) 3_765 ? 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 C15 Mo1 C13 87.28(10) . . ? C15 Mo1 C14 85.54(11) . . ? C13 Mo1 C14 85.88(11) . . ? C15 Mo1 N2 173.94(9) . . ? C13 Mo1 N2 98.75(9) . . ? C14 Mo1 N2 95.40(10) . . ? C15 Mo1 N1 101.65(9) . . ? C13 Mo1 N1 171.06(9) . . ? C14 Mo1 N1 94.37(9) . . ? N2 Mo1 N1 72.32(8) . . ? C15 Mo1 P1 88.80(8) . . ? C13 Mo1 P1 88.26(8) . . ? C14 Mo1 P1 172.04(8) . . ? N2 Mo1 P1 90.81(6) . . ? N1 Mo1 P1 92.25(6) . . ? C30 P1 C40 103.20(12) . . ? C30 P1 C20 104.57(12) . . ? C40 P1 C20 98.65(11) . . ? C30 P1 Mo1 112.60(9) . . ? C40 P1 Mo1 120.11(9) . . ? C20 P1 Mo1 115.60(9) . . ? C4 O1 H1 110(8) . . ? C4 O1 H1X 127.1(2) . . ? H1 O1 H1X 123(8) . . ? C7 N1 C1 118.6(2) . . ? C7 N1 Mo1 116.28(18) . . ? C1 N1 Mo1 125.14(15) . . ? C12 N2 C8 116.6(2) . . ? C12 N2 Mo1 126.58(16) . . ? C8 N2 Mo1 116.81(17) . . ? C2 C1 C6 119.2(2) . . ? C2 C1 N1 118.8(2) . . ? C6 C1 N1 121.9(2) . . ? C1 C2 C3 121.3(2) . . ? C1 C2 H2 115.7(19) . . ? C3 C2 H2 123.0(19) . . ? C2 C3 C4 119.1(2) . . ? C2 C3 H3 120.0(15) . . ? C4 C3 H3 120.8(15) . . ? O1 C4 C5 120.0(2) . . ? O1 C4 C3 119.5(2) . . ? C5 C4 C3 120.5(2) . . ? C4 C5 C6 120.0(2) . . ? C4 C5 H5 121(2) . . ? C6 C5 H5 119(2) . . ? C5 C6 C1 119.9(3) . . ? C5 C6 H6 120(2) . . ? C1 C6 H6 119.7(19) . . ? N1 C7 C8 119.2(2) . . ? N1 C7 H7 123.5(17) . . ? C8 C7 H7 117.3(17) . . ? N2 C8 C9 123.0(3) . . ? N2 C8 C7 115.3(2) . . ? C9 C8 C7 121.7(2) . . ? C10 C9 C8 119.0(3) . . ? C10 C9 H9 120.9(18) . . ? C8 C9 H9 119.9(18) . . ? C11 C10 C9 118.1(3) . . ? C11 C10 H10 115.4(15) . . ? C9 C10 H10 125.8(16) . . ? C12 C11 C10 119.9(3) . . ? C12 C11 H11 122(2) . . ? C10 C11 H11 118(2) . . ? N2 C12 C11 123.4(3) . . ? N2 C12 H12 112.8(19) . . ? C11 C12 H12 123(2) . . ? O13 C13 Mo1 178.0(2) . . ? O14 C14 Mo1 173.6(2) . . ? O15 C15 Mo1 178.8(2) . . ? C21 C20 C25 118.4(2) . . ? C21 C20 P1 118.0(2) . . ? C25 C20 P1 123.5(2) . . ? C20 C21 C22 121.3(3) . . ? C20 C21 H21 121.3(16) . . ? C22 C21 H21 117.3(16) . . ? C23 C22 C21 119.7(3) . . ? C23 C22 H22 120.7(17) . . ? C21 C22 H22 119.6(17) . . ? C22 C23 C24 120.2(3) . . ? C22 C23 H23 118(2) . . ? C24 C23 H23 122(2) . . ? C23 C24 C25 119.5(3) . . ? C23 C24 H24 122(2) . . ? C25 C24 H24 118(2) . . ? C20 C25 C24 120.8(3) . . ? C20 C25 H25 110.9(19) . . ? C24 C25 H25 127.5(19) . . ? C35 C30 C31 118.3(3) . . ? C35 C30 P1 120.21(19) . . ? C31 C30 P1 121.0(2) . . ? C32 C31 C30 120.3(3) . . ? C32 C31 H31 122.9(19) . . ? C30 C31 H31 116.3(19) . . ? C33 C32 C31 120.7(3) . . ? C33 C32 H32 121.2(18) . . ? C31 C32 H32 118.1(18) . . ? C32 C33 C34 119.3(3) . . ? C32 C33 H33 120.0(18) . . ? C34 C33 H33 120.6(18) . . ? C35 C34 C33 119.8(3) . . ? C35 C34 H34 119.8(19) . . ? C33 C34 H34 120.3(19) . . ? C30 C35 C34 121.5(3) . . ? C30 C35 H35 117(2) . . ? C34 C35 H35 121(2) . . ? C41 C40 C45 118.8(2) . . ? C41 C40 P1 121.1(2) . . ? C45 C40 P1 120.0(2) . . ? C40 C41 C42 120.1(3) . . ? C40 C41 H41 109.5(2) . . ? C42 C41 H41 130.1(3) . . ? C43 C42 C41 120.9(3) . . ? C43 C42 H42 124.1(18) . . ? C41 C42 H42 115.0(18) . . ? C42 C43 C44 119.6(3) . . ? C42 C43 H43 120.6(18) . . ? C44 C43 H43 119.8(18) . . ? C45 C44 C43 120.1(3) . . ? C45 C44 H44 115.1(17) . . ? C43 C44 H44 124.5(17) . . ? C44 C45 C40 120.5(3) . . ? C44 C45 H45 118.7(16) . . ? C40 C45 H45 120.8(16) . . ? C101 O100 C102 74.0(8) 3_765 . ? C101 O100 C101 92.3(9) 3_765 . ? C102 O100 C101 102.7(8) . . ? C101 O100 H1X 114.8(8) 3_765 . ? C102 O100 H1X 122.4(4) . . ? C101 O100 H1X 131.6(8) . . ? C103 C100 C102 27(2) 3_765 3_765 ? C103 C100 C101 61(2) 3_765 . ? C102 C100 C101 67.0(7) 3_765 . ? O100 C101 C103 94.3(12) 3_765 3_765 ? O100 C101 O100 87.7(9) 3_765 . ? C103 C101 O100 98.5(11) 3_765 . ? O100 C101 C100 109.3(11) 3_765 . ? C103 C101 C100 18.3(7) 3_765 . ? O100 C101 C100 108.7(10) . . ? O100 C101 C102 55.1(7) 3_765 3_765 ? C103 C101 C102 39.4(7) 3_765 3_765 ? O100 C101 C102 99.0(9) . 3_765 ? C100 C101 C102 54.5(7) . 3_765 ? C103 C102 O100 106.0(11) . . ? C103 C102 C100 12.3(9) . 3_765 ? O100 C102 C100 109.0(6) . 3_765 ? C103 C102 C101 55.4(10) . 3_765 ? O100 C102 C101 50.9(6) . 3_765 ? C100 C102 C101 58.5(7) 3_765 3_765 ? C100 C103 C102 140(3) 3_765 . ? C100 C103 C101 100(3) 3_765 3_765 ? C102 C103 C101 85.3(13) . 3_765 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 Mo1 P1 C30 174.33(11) . . . . ? C13 Mo1 P1 C30 -98.35(12) . . . . ? C14 Mo1 P1 C30 -141.0(6) . . . . ? N2 Mo1 P1 C30 0.39(10) . . . . ? N1 Mo1 P1 C30 72.72(10) . . . . ? C15 Mo1 P1 C40 52.51(11) . . . . ? C13 Mo1 P1 C40 139.83(12) . . . . ? C14 Mo1 P1 C40 97.2(6) . . . . ? N2 Mo1 P1 C40 -121.44(10) . . . . ? N1 Mo1 P1 C40 -49.10(10) . . . . ? C15 Mo1 P1 C20 -65.57(12) . . . . ? C13 Mo1 P1 C20 21.75(13) . . . . ? C14 Mo1 P1 C20 -20.9(6) . . . . ? N2 Mo1 P1 C20 120.48(11) . . . . ? N1 Mo1 P1 C20 -167.18(11) . . . . ? C15 Mo1 N1 C7 -177.34(19) . . . . ? C13 Mo1 N1 C7 5.0(7) . . . . ? C14 Mo1 N1 C7 96.3(2) . . . . ? N2 Mo1 N1 C7 2.04(18) . . . . ? P1 Mo1 N1 C7 -88.10(18) . . . . ? C15 Mo1 N1 C1 2.9(2) . . . . ? C13 Mo1 N1 C1 -174.8(6) . . . . ? C14 Mo1 N1 C1 -83.5(2) . . . . ? N2 Mo1 N1 C1 -177.8(2) . . . . ? P1 Mo1 N1 C1 92.10(19) . . . . ? C15 Mo1 N2 C12 -175.7(8) . . . . ? C13 Mo1 N2 C12 -1.0(2) . . . . ? C14 Mo1 N2 C12 85.6(2) . . . . ? N1 Mo1 N2 C12 178.5(2) . . . . ? P1 Mo1 N2 C12 -89.4(2) . . . . ? C15 Mo1 N2 C8 3.0(10) . . . . ? C13 Mo1 N2 C8 177.63(19) . . . . ? C14 Mo1 N2 C8 -95.72(19) . . . . ? N1 Mo1 N2 C8 -2.84(17) . . . . ? P1 Mo1 N2 C8 89.27(18) . . . . ? C7 N1 C1 C2 -145.5(2) . . . . ? Mo1 N1 C1 C2 34.3(3) . . . . ? C7 N1 C1 C6 37.8(4) . . . . ? Mo1 N1 C1 C6 -142.4(2) . . . . ? C6 C1 C2 C3 0.4(4) . . . . ? N1 C1 C2 C3 -176.4(2) . . . . ? C1 C2 C3 C4 0.6(4) . . . . ? C2 C3 C4 O1 178.8(2) . . . . ? C2 C3 C4 C5 -1.1(4) . . . . ? O1 C4 C5 C6 -179.4(3) . . . . ? C3 C4 C5 C6 0.6(4) . . . . ? C4 C5 C6 C1 0.5(4) . . . . ? C2 C1 C6 C5 -1.0(4) . . . . ? N1 C1 C6 C5 175.7(2) . . . . ? C1 N1 C7 C8 178.7(2) . . . . ? Mo1 N1 C7 C8 -1.1(3) . . . . ? C12 N2 C8 C9 0.7(4) . . . . ? Mo1 N2 C8 C9 -178.1(2) . . . . ? C12 N2 C8 C7 -177.9(2) . . . . ? Mo1 N2 C8 C7 3.3(3) . . . . ? N1 C7 C8 N2 -1.5(4) . . . . ? N1 C7 C8 C9 179.9(3) . . . . ? N2 C8 C9 C10 -0.5(4) . . . . ? C7 C8 C9 C10 178.0(3) . . . . ? C8 C9 C10 C11 -0.2(4) . . . . ? C9 C10 C11 C12 0.6(5) . . . . ? C8 N2 C12 C11 -0.2(4) . . . . ? Mo1 N2 C12 C11 178.5(2) . . . . ? C10 C11 C12 N2 -0.5(5) . . . . ? C15 Mo1 C13 O13 -33(7) . . . . ? C14 Mo1 C13 O13 52(7) . . . . ? N2 Mo1 C13 O13 147(7) . . . . ? N1 Mo1 C13 O13 144(7) . . . . ? P1 Mo1 C13 O13 -122(7) . . . . ? C15 Mo1 C14 O14 24(2) . . . . ? C13 Mo1 C14 O14 -63(2) . . . . ? N2 Mo1 C14 O14 -162(2) . . . . ? N1 Mo1 C14 O14 126(2) . . . . ? P1 Mo1 C14 O14 -21(3) . . . . ? C13 Mo1 C15 O15 41(11) . . . . ? C14 Mo1 C15 O15 -45(11) . . . . ? N2 Mo1 C15 O15 -144(11) . . . . ? N1 Mo1 C15 O15 -139(11) . . . . ? P1 Mo1 C15 O15 129(11) . . . . ? C30 P1 C20 C21 170.2(2) . . . . ? C40 P1 C20 C21 -83.7(2) . . . . ? Mo1 P1 C20 C21 45.8(2) . . . . ? C30 P1 C20 C25 -14.2(3) . . . . ? C40 P1 C20 C25 91.9(3) . . . . ? Mo1 P1 C20 C25 -138.6(2) . . . . ? C25 C20 C21 C22 -0.8(4) . . . . ? P1 C20 C21 C22 175.0(2) . . . . ? C20 C21 C22 C23 1.2(4) . . . . ? C21 C22 C23 C24 -0.5(5) . . . . ? C22 C23 C24 C25 -0.6(5) . . . . ? C21 C20 C25 C24 -0.3(5) . . . . ? P1 C20 C25 C24 -175.9(3) . . . . ? C23 C24 C25 C20 1.0(5) . . . . ? C40 P1 C30 C35 -155.9(2) . . . . ? C20 P1 C30 C35 -53.2(2) . . . . ? Mo1 P1 C30 C35 73.1(2) . . . . ? C40 P1 C30 C31 32.4(2) . . . . ? C20 P1 C30 C31 135.1(2) . . . . ? Mo1 P1 C30 C31 -98.6(2) . . . . ? C35 C30 C31 C32 2.1(4) . . . . ? P1 C30 C31 C32 174.0(2) . . . . ? C30 C31 C32 C33 0.1(5) . . . . ? C31 C32 C33 C34 -1.3(5) . . . . ? C32 C33 C34 C35 0.3(5) . . . . ? C31 C30 C35 C34 -3.1(4) . . . . ? P1 C30 C35 C34 -175.0(2) . . . . ? C33 C34 C35 C30 1.9(5) . . . . ? C30 P1 C40 C41 -131.3(2) . . . . ? C20 P1 C40 C41 121.4(2) . . . . ? Mo1 P1 C40 C41 -5.0(2) . . . . ? C30 P1 C40 C45 51.1(2) . . . . ? C20 P1 C40 C45 -56.2(2) . . . . ? Mo1 P1 C40 C45 177.39(16) . . . . ? C45 C40 C41 C42 -0.7(4) . . . . ? P1 C40 C41 C42 -178.4(2) . . . . ? C40 C41 C42 C43 0.7(4) . . . . ? C41 C42 C43 C44 -0.5(4) . . . . ? C42 C43 C44 C45 0.4(4) . . . . ? C43 C44 C45 C40 -0.4(4) . . . . ? C41 C40 C45 C44 0.6(4) . . . . ? P1 C40 C45 C44 178.3(2) . . . . ? C101 O100 C101 O100 0.000(1) 3_765 . . 3_765 ? C102 O100 C101 O100 74.1(8) . . . 3_765 ? C101 O100 C101 C103 94.0(13) 3_765 . . 3_765 ? C102 O100 C101 C103 168.1(9) . . . 3_765 ? C101 O100 C101 C100 109.6(13) 3_765 . . . ? C102 O100 C101 C100 -176.3(8) . . . . ? C101 O100 C101 C102 54.2(7) 3_765 . . 3_765 ? C102 O100 C101 C102 128.2(7) . . . 3_765 ? C103 C100 C101 O100 36(3) 3_765 . . 3_765 ? C102 C100 C101 O100 6.5(8) 3_765 . . 3_765 ? C102 C100 C101 C103 -30(2) 3_765 . . 3_765 ? C103 C100 C101 O100 -58(3) 3_765 . . . ? C102 C100 C101 O100 -87.7(10) 3_765 . . . ? C103 C100 C101 C102 30(2) 3_765 . . 3_765 ? C101 O100 C102 C103 5.7(12) 3_765 . . . ? C101 O100 C102 C103 -83.0(12) . . . . ? C101 O100 C102 C100 -6.8(8) 3_765 . . 3_765 ? C101 O100 C102 C100 -95.5(9) . . . 3_765 ? C101 O100 C102 C101 -88.7(10) . . . 3_765 ? O100 C102 C103 C100 -106(5) . . . 3_765 ? C101 C102 C103 C100 -101(5) 3_765 . . 3_765 ? O100 C102 C103 C101 -5.4(11) . . . 3_765 ? C100 C102 C103 C101 101(5) 3_765 . . 3_765 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 32.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.241 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.097 #===END # 1. SUBMISSION DETAILS #============================================================================== data_ka291 _database_code_CSD 168310 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H25 Mo N2 O4 P' _chemical_formula_weight 640.46 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' 'P' 'P' 0.1023 0.0942 '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 monoklin _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.464(3) _cell_length_b 9.6760(19) _cell_length_c 18.523(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.89(3) _cell_angle_gamma 90.00 _cell_volume 2851.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.80 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type 'experimentell' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _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 'NONIUS KAPPA CCD' _diffrn_measurement_method 'O-Scan ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19266 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 32.07 _reflns_number_total 9904 _reflns_number_gt 7035 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0652P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9904 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1310 _refine_ls_wR_factor_gt 0.1185 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.151 _refine_ls_shift/su_mean 0.005 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.846201(12) 0.287141(18) 0.537134(10) 0.02999(7) Uani 1 1 d . . . P1 P 0.69356(4) 0.20610(5) 0.51851(3) 0.03132(13) Uani 1 1 d . . . O1 O 0.79597(14) 0.26929(19) 0.14349(10) 0.0422(4) Uani 1 1 d . . . O13 O 0.84181(13) 0.4696(2) 0.67422(10) 0.0546(5) Uani 1 1 d . . . O14 O 1.02881(13) 0.4058(2) 0.57436(11) 0.0596(5) Uani 1 1 d . . . O15 O 0.78985(13) 0.55998(17) 0.45047(9) 0.0461(4) Uani 1 1 d . . . N1 N 0.86045(12) 0.13834(18) 0.44603(10) 0.0321(4) Uani 1 1 d . . . N2 N 0.89131(12) 0.0822(2) 0.59151(10) 0.0365(4) Uani 1 1 d . . . C1 C 0.84462(14) 0.1683(2) 0.36793(12) 0.0314(4) Uani 1 1 d . . . C2 C 0.86722(16) 0.2962(2) 0.34549(13) 0.0335(5) Uani 1 1 d . . . C3 C 0.85248(16) 0.3276(2) 0.27027(13) 0.0338(5) Uani 1 1 d . . . C4 C 0.81209(16) 0.2321(2) 0.21679(13) 0.0347(5) Uani 1 1 d . . . C5 C 0.78895(17) 0.1038(2) 0.23892(13) 0.0382(5) Uani 1 1 d . . . C6 C 0.80554(16) 0.0722(2) 0.31411(13) 0.0367(5) Uani 1 1 d . . . C7 C 0.88465(16) 0.0144(2) 0.46749(14) 0.0387(5) Uani 1 1 d . . . C8 C 0.90175(15) -0.0218(2) 0.54540(13) 0.0387(5) Uani 1 1 d . . . C9 C 0.92579(18) -0.1554(3) 0.57076(17) 0.0486(6) Uani 1 1 d . . . C10 C 0.94081(19) -0.1828(3) 0.64595(18) 0.0550(7) Uani 1 1 d . . . C11 C 0.9330(2) -0.0790(3) 0.69289(17) 0.0563(8) Uani 1 1 d . . . C12 C 0.90777(18) 0.0528(3) 0.66471(15) 0.0474(6) Uani 1 1 d . . . C13 C 0.84122(16) 0.3968(2) 0.62394(12) 0.0374(5) Uani 1 1 d . . . C14 C 0.96232(17) 0.3584(2) 0.55833(12) 0.0393(5) Uani 1 1 d . . . C15 C 0.81061(15) 0.4550(2) 0.48173(12) 0.0332(5) Uani 1 1 d . . . C20 C 0.61899(16) 0.3032(2) 0.55786(13) 0.0350(5) Uani 1 1 d . . . C21 C 0.62834(18) 0.4450(3) 0.56956(14) 0.0416(5) Uani 1 1 d . . . C22 C 0.5679(2) 0.5198(3) 0.59278(16) 0.0509(7) Uani 1 1 d . . . C23 C 0.4984(2) 0.4548(3) 0.60524(16) 0.0515(7) Uani 1 1 d . . . C24 C 0.4889(2) 0.3144(3) 0.59520(18) 0.0522(7) Uani 1 1 d . . . C25 C 0.54886(19) 0.2397(3) 0.57178(17) 0.0471(6) Uani 1 1 d . . . C30 C 0.69285(14) 0.0363(2) 0.56104(13) 0.0330(5) Uani 1 1 d . . . C31 C 0.70190(18) 0.0259(3) 0.63746(14) 0.0421(6) Uani 1 1 d . . . C32 C 0.7156(2) -0.1011(3) 0.67267(16) 0.0500(7) Uani 1 1 d . . . C33 C 0.7212(2) -0.2196(3) 0.6322(2) 0.0523(7) Uani 1 1 d . . . C34 C 0.7114(2) -0.2099(3) 0.5567(2) 0.0568(8) Uani 1 1 d . . . C35 C 0.69808(19) -0.0839(3) 0.52066(16) 0.0468(6) Uani 1 1 d . . . C40 C 0.63072(16) 0.1858(2) 0.42128(13) 0.0352(5) Uani 1 1 d . . . C41 C 0.65218(16) 0.2619(3) 0.36568(13) 0.0363(5) Uani 1 1 d . . . C42 C 0.60467(17) 0.2528(3) 0.29199(13) 0.0412(6) Uani 1 1 d . . . C43 C 0.53590(18) 0.1660(3) 0.27359(15) 0.0467(6) Uani 1 1 d . . . C44 C 0.5136(2) 0.0905(4) 0.32861(16) 0.0597(8) Uani 1 1 d . . . C45 C 0.5603(2) 0.0997(3) 0.40242(16) 0.0555(8) Uani 1 1 d . . . H1 H 0.767(2) 0.223(3) 0.1235(17) 0.038(9) Uiso 1 1 d . . . H2 H 0.8932(15) 0.363(3) 0.3804(13) 0.033(6) Uiso 1 1 d . . . H3 H 0.8679(19) 0.419(3) 0.2569(16) 0.059(8) Uiso 1 1 d . . . H5 H 0.7559(17) 0.044(3) 0.2016(15) 0.047(8) Uiso 1 1 d . . . H6 H 0.7842(17) -0.015(3) 0.3304(14) 0.043(7) Uiso 1 1 d . . . H7 H 0.8933(16) -0.052(3) 0.4317(14) 0.042(7) Uiso 1 1 d . . . H9 H 0.928(2) -0.212(3) 0.5359(18) 0.055(10) Uiso 1 1 d . . . H10 H 0.955(2) -0.283(3) 0.6703(17) 0.057(9) Uiso 1 1 d . . . H11 H 0.938(2) -0.088(3) 0.7445(18) 0.066(10) Uiso 1 1 d . . . H12 H 0.8977(18) 0.130(3) 0.6938(15) 0.052(8) Uiso 1 1 d . . . H21 H 0.6754(16) 0.487(3) 0.5621(13) 0.034(7) Uiso 1 1 d . . . H22 H 0.570(2) 0.631(4) 0.6021(18) 0.071(10) Uiso 1 1 d . . . H23 H 0.453(2) 0.501(4) 0.6190(18) 0.075(10) Uiso 1 1 d . . . H24 H 0.437(2) 0.303(3) 0.604(2) 0.072(12) Uiso 1 1 d . . . H25 H 0.5440(17) 0.135(3) 0.5682(14) 0.049(8) Uiso 1 1 d . . . H31 H 0.6997(13) 0.106(2) 0.6664(11) 0.018(5) Uiso 1 1 d . . . H32 H 0.724(2) -0.109(4) 0.7232(18) 0.069(10) Uiso 1 1 d . . . H33 H 0.730(2) -0.312(3) 0.6555(17) 0.060(9) Uiso 1 1 d . . . H34 H 0.713(2) -0.288(4) 0.526(2) 0.080(12) Uiso 1 1 d . . . H35 H 0.687(2) -0.076(3) 0.4668(17) 0.062(9) Uiso 1 1 d . . . H41 H 0.7022(15) 0.322(2) 0.3821(12) 0.026(6) Uiso 1 1 d . . . H42 H 0.6217(16) 0.309(3) 0.2545(14) 0.034(7) Uiso 1 1 d . . . H43 H 0.508(2) 0.159(4) 0.2200(18) 0.071(10) Uiso 1 1 d . . . H44 H 0.471(2) 0.031(3) 0.3183(16) 0.059(9) Uiso 1 1 d . . . H45 H 0.5452(18) 0.036(3) 0.4389(15) 0.049(8) Uiso 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 0.03231(12) 0.02965(10) 0.02684(11) 0.00035(6) 0.00547(7) -0.00454(7) P1 0.0341(3) 0.0289(3) 0.0314(3) -0.00159(19) 0.0092(2) -0.0040(2) O1 0.0582(13) 0.0371(9) 0.0318(9) -0.0014(7) 0.0128(8) -0.0044(8) O13 0.0664(14) 0.0585(11) 0.0361(9) -0.0088(8) 0.0082(9) 0.0101(10) O14 0.0446(11) 0.0752(14) 0.0566(12) -0.0029(10) 0.0087(9) -0.0254(10) O15 0.0608(12) 0.0364(8) 0.0418(9) 0.0045(7) 0.0147(8) 0.0054(8) N1 0.0323(10) 0.0319(9) 0.0321(9) -0.0005(7) 0.0081(7) -0.0054(7) N2 0.0321(10) 0.0398(10) 0.0353(10) 0.0054(8) 0.0049(8) -0.0050(8) C1 0.0320(11) 0.0317(9) 0.0310(10) -0.0025(8) 0.0092(8) -0.0020(8) C2 0.0338(12) 0.0326(10) 0.0348(11) -0.0048(8) 0.0104(9) -0.0032(9) C3 0.0373(13) 0.0296(9) 0.0361(11) -0.0004(8) 0.0124(9) -0.0020(9) C4 0.0417(14) 0.0316(11) 0.0335(11) -0.0014(8) 0.0146(10) 0.0005(9) C5 0.0496(15) 0.0309(10) 0.0351(12) -0.0065(8) 0.0128(10) -0.0057(10) C6 0.0457(14) 0.0274(10) 0.0376(12) -0.0028(8) 0.0119(10) -0.0030(9) C7 0.0421(14) 0.0322(11) 0.0410(12) 0.0002(9) 0.0093(10) 0.0030(10) C8 0.0333(13) 0.0369(11) 0.0447(13) 0.0082(9) 0.0080(10) 0.0033(9) C9 0.0454(16) 0.0426(14) 0.0566(17) 0.0106(12) 0.0113(13) 0.0078(12) C10 0.0489(17) 0.0501(15) 0.0657(19) 0.0227(14) 0.0138(14) 0.0115(13) C11 0.0525(18) 0.0669(19) 0.0457(16) 0.0246(14) 0.0059(13) 0.0043(14) C12 0.0475(16) 0.0519(15) 0.0398(13) 0.0114(11) 0.0056(11) 0.0010(12) C13 0.0403(13) 0.0396(11) 0.0299(11) 0.0021(9) 0.0047(9) -0.0014(10) C14 0.0439(14) 0.0404(12) 0.0333(11) -0.0015(9) 0.0094(10) -0.0080(10) C15 0.0389(13) 0.0325(10) 0.0278(10) -0.0024(8) 0.0081(9) -0.0040(9) C20 0.0384(13) 0.0340(11) 0.0338(11) 0.0007(8) 0.0115(9) 0.0018(9) C21 0.0454(15) 0.0337(11) 0.0465(14) -0.0019(10) 0.0132(11) -0.0004(10) C22 0.0604(19) 0.0383(13) 0.0543(16) -0.0046(11) 0.0152(14) 0.0064(12) C23 0.0496(17) 0.0563(16) 0.0508(16) -0.0012(12) 0.0166(13) 0.0161(14) C24 0.0419(16) 0.0591(17) 0.0598(18) -0.0017(13) 0.0209(14) 0.0004(13) C25 0.0477(17) 0.0394(13) 0.0582(17) -0.0052(11) 0.0207(13) -0.0030(12) C30 0.0307(11) 0.0296(10) 0.0407(12) -0.0019(8) 0.0126(9) -0.0037(8) C31 0.0516(16) 0.0365(12) 0.0387(13) -0.0016(9) 0.0128(11) -0.0023(11) C32 0.0579(18) 0.0471(14) 0.0452(15) 0.0100(11) 0.0132(13) -0.0006(12) C33 0.0507(18) 0.0362(13) 0.073(2) 0.0124(12) 0.0215(15) 0.0004(11) C34 0.076(2) 0.0332(13) 0.072(2) -0.0040(12) 0.0375(18) -0.0014(13) C35 0.0625(18) 0.0364(12) 0.0469(15) -0.0075(10) 0.0238(13) -0.0068(11) C40 0.0357(13) 0.0365(11) 0.0326(11) -0.0047(8) 0.0068(9) -0.0041(9) C41 0.0342(13) 0.0381(11) 0.0360(12) -0.0030(9) 0.0083(10) -0.0021(9) C42 0.0427(15) 0.0465(12) 0.0332(13) 0.0023(10) 0.0078(11) 0.0048(11) C43 0.0448(15) 0.0530(15) 0.0371(13) -0.0046(11) 0.0010(11) 0.0044(12) C44 0.0507(18) 0.076(2) 0.0459(16) -0.0030(14) 0.0007(13) -0.0273(16) C45 0.0521(17) 0.0685(18) 0.0420(14) 0.0033(13) 0.0049(12) -0.0264(14) _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 C15 1.930(2) . ? Mo1 C13 1.946(2) . ? Mo1 C14 1.974(3) . ? Mo1 N2 2.2617(19) . ? Mo1 N1 2.2758(18) . ? Mo1 P1 2.5699(8) . ? P1 C30 1.824(2) . ? P1 C20 1.839(3) . ? P1 C40 1.843(2) . ? O1 C4 1.363(3) . ? O1 H1 0.69(3) . ? O13 C13 1.166(3) . ? O14 C14 1.153(3) . ? O15 C15 1.176(3) . ? N1 C7 1.294(3) . ? N1 C1 1.432(3) . ? N2 C12 1.343(3) . ? N2 C8 1.359(3) . ? C1 C2 1.387(3) . ? C1 C6 1.394(3) . ? C2 C3 1.385(3) . ? C2 H2 0.94(2) . ? C3 C4 1.393(3) . ? C3 H3 0.97(3) . ? C4 C5 1.391(3) . ? C5 C6 1.383(3) . ? C5 H5 0.95(3) . ? C6 H6 0.99(3) . ? C7 C8 1.441(3) . ? C7 H7 0.96(3) . ? C8 C9 1.397(3) . ? C9 C10 1.376(4) . ? C9 H9 0.85(3) . ? C10 C11 1.356(5) . ? C10 H10 1.07(3) . ? C11 C12 1.400(4) . ? C11 H11 0.94(3) . ? C12 H12 0.96(3) . ? C20 C25 1.389(4) . ? C20 C21 1.391(3) . ? C21 C22 1.386(4) . ? C21 H21 0.92(3) . ? C22 C23 1.376(4) . ? C22 H22 1.08(4) . ? C23 C24 1.374(4) . ? C23 H23 0.96(4) . ? C24 C25 1.380(4) . ? C24 H24 0.92(4) . ? C25 H25 1.01(3) . ? C30 C31 1.388(3) . ? C30 C35 1.397(3) . ? C31 C32 1.382(4) . ? C31 H31 0.95(2) . ? C32 C33 1.386(4) . ? C32 H32 0.91(3) . ? C33 C34 1.369(5) . ? C33 H33 0.99(3) . ? C34 C35 1.380(4) . ? C34 H34 0.95(4) . ? C35 H35 0.97(3) . ? C40 C41 1.383(3) . ? C40 C45 1.397(4) . ? C41 C42 1.391(3) . ? C41 H41 0.99(2) . ? C42 C43 1.380(4) . ? C42 H42 0.98(3) . ? C43 C44 1.378(4) . ? C43 H43 0.98(3) . ? C44 C45 1.388(4) . ? C44 H44 0.89(3) . ? C45 H45 0.99(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 C15 Mo1 C13 84.77(9) . . ? C15 Mo1 C14 87.60(10) . . ? C13 Mo1 C14 83.66(10) . . ? C15 Mo1 N2 174.14(8) . . ? C13 Mo1 N2 100.91(9) . . ? C14 Mo1 N2 91.56(9) . . ? C15 Mo1 N1 102.30(8) . . ? C13 Mo1 N1 172.78(8) . . ? C14 Mo1 N1 95.12(9) . . ? N2 Mo1 N1 71.99(7) . . ? C15 Mo1 P1 91.87(7) . . ? C13 Mo1 P1 91.71(8) . . ? C14 Mo1 P1 175.37(7) . . ? N2 Mo1 P1 89.43(5) . . ? N1 Mo1 P1 89.49(5) . . ? C30 P1 C20 102.13(10) . . ? C30 P1 C40 105.18(10) . . ? C20 P1 C40 100.23(12) . . ? C30 P1 Mo1 109.37(8) . . ? C20 P1 Mo1 121.36(8) . . ? C40 P1 Mo1 116.60(9) . . ? C4 O1 H1 107(3) . . ? C7 N1 C1 117.36(19) . . ? C7 N1 Mo1 116.16(16) . . ? C1 N1 Mo1 126.48(14) . . ? C12 N2 C8 116.9(2) . . ? C12 N2 Mo1 126.37(18) . . ? C8 N2 Mo1 116.71(14) . . ? C2 C1 C6 119.4(2) . . ? C2 C1 N1 119.35(19) . . ? C6 C1 N1 121.2(2) . . ? C3 C2 C1 120.4(2) . . ? C3 C2 H2 118.2(15) . . ? C1 C2 H2 121.4(14) . . ? C2 C3 C4 119.9(2) . . ? C2 C3 H3 117.8(17) . . ? C4 C3 H3 122.2(17) . . ? O1 C4 C5 122.1(2) . . ? O1 C4 C3 117.9(2) . . ? C5 C4 C3 120.0(2) . . ? C6 C5 C4 119.7(2) . . ? C6 C5 H5 121.7(16) . . ? C4 C5 H5 118.2(16) . . ? C5 C6 C1 120.6(2) . . ? C5 C6 H6 120.1(15) . . ? C1 C6 H6 119.0(15) . . ? N1 C7 C8 119.9(2) . . ? N1 C7 H7 119.9(16) . . ? C8 C7 H7 120.1(15) . . ? N2 C8 C9 123.0(2) . . ? N2 C8 C7 115.2(2) . . ? C9 C8 C7 121.8(2) . . ? C10 C9 C8 118.7(3) . . ? C10 C9 H9 128(2) . . ? C8 C9 H9 114(2) . . ? C11 C10 C9 119.0(3) . . ? C11 C10 H10 116.7(17) . . ? C9 C10 H10 124.2(17) . . ? C10 C11 C12 120.2(3) . . ? C10 C11 H11 126(2) . . ? C12 C11 H11 114(2) . . ? N2 C12 C11 122.2(3) . . ? N2 C12 H12 112.6(17) . . ? C11 C12 H12 125.1(17) . . ? O13 C13 Mo1 175.1(2) . . ? O14 C14 Mo1 175.3(2) . . ? O15 C15 Mo1 177.46(18) . . ? C25 C20 C21 118.1(2) . . ? C25 C20 P1 121.28(19) . . ? C21 C20 P1 120.5(2) . . ? C22 C21 C20 120.3(3) . . ? C22 C21 H21 121.0(17) . . ? C20 C21 H21 118.8(17) . . ? C23 C22 C21 120.6(3) . . ? C23 C22 H22 114.7(18) . . ? C21 C22 H22 124.8(18) . . ? C24 C23 C22 119.9(3) . . ? C24 C23 H23 115(2) . . ? C22 C23 H23 125(2) . . ? C23 C24 C25 119.7(3) . . ? C23 C24 H24 100(2) . . ? C25 C24 H24 140(2) . . ? C24 C25 C20 121.5(3) . . ? C24 C25 H25 119.5(16) . . ? C20 C25 H25 118.9(16) . . ? C31 C30 C35 118.7(2) . . ? C31 C30 P1 119.64(17) . . ? C35 C30 P1 120.70(18) . . ? C32 C31 C30 120.5(2) . . ? C32 C31 H31 119.0(13) . . ? C30 C31 H31 120.6(13) . . ? C31 C32 C33 120.4(3) . . ? C31 C32 H32 121(2) . . ? C33 C32 H32 118(2) . . ? C34 C33 C32 119.3(2) . . ? C34 C33 H33 118.3(18) . . ? C32 C33 H33 122.3(18) . . ? C33 C34 C35 121.1(3) . . ? C33 C34 H34 123(2) . . ? C35 C34 H34 116(2) . . ? C34 C35 C30 120.0(2) . . ? C34 C35 H35 122.4(19) . . ? C30 C35 H35 117.4(19) . . ? C41 C40 C45 119.0(2) . . ? C41 C40 P1 118.96(18) . . ? C45 C40 P1 121.95(19) . . ? C40 C41 C42 120.7(2) . . ? C40 C41 H41 115.9(13) . . ? C42 C41 H41 123.4(13) . . ? C43 C42 C41 120.0(2) . . ? C43 C42 H42 121.9(15) . . ? C41 C42 H42 118.2(15) . . ? C44 C43 C42 119.8(2) . . ? C44 C43 H43 125(2) . . ? C42 C43 H43 116(2) . . ? C43 C44 C45 120.6(3) . . ? C43 C44 H44 122.0(19) . . ? C45 C44 H44 117.3(19) . . ? C44 C45 C40 119.9(3) . . ? C44 C45 H45 117.4(16) . . ? C40 C45 H45 122.4(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 Mo1 P1 C30 177.96(10) . . . . ? C13 Mo1 P1 C30 -97.21(10) . . . . ? C14 Mo1 P1 C30 -98.7(9) . . . . ? N2 Mo1 P1 C30 3.68(9) . . . . ? N1 Mo1 P1 C30 75.67(9) . . . . ? C15 Mo1 P1 C20 -63.67(11) . . . . ? C13 Mo1 P1 C20 21.15(11) . . . . ? C14 Mo1 P1 C20 19.6(9) . . . . ? N2 Mo1 P1 C20 122.05(10) . . . . ? N1 Mo1 P1 C20 -165.96(10) . . . . ? C15 Mo1 P1 C40 58.86(10) . . . . ? C13 Mo1 P1 C40 143.69(11) . . . . ? C14 Mo1 P1 C40 142.2(9) . . . . ? N2 Mo1 P1 C40 -115.42(10) . . . . ? N1 Mo1 P1 C40 -43.43(9) . . . . ? C15 Mo1 N1 C7 179.76(18) . . . . ? C13 Mo1 N1 C7 11.2(8) . . . . ? C14 Mo1 N1 C7 91.11(19) . . . . ? N2 Mo1 N1 C7 1.13(17) . . . . ? P1 Mo1 N1 C7 -88.44(18) . . . . ? C15 Mo1 N1 C1 -0.83(19) . . . . ? C13 Mo1 N1 C1 -169.4(6) . . . . ? C14 Mo1 N1 C1 -89.48(19) . . . . ? N2 Mo1 N1 C1 -179.46(19) . . . . ? P1 Mo1 N1 C1 90.97(17) . . . . ? C15 Mo1 N2 C12 166.2(8) . . . . ? C13 Mo1 N2 C12 0.7(2) . . . . ? C14 Mo1 N2 C12 84.5(2) . . . . ? N1 Mo1 N2 C12 179.4(2) . . . . ? P1 Mo1 N2 C12 -91.0(2) . . . . ? C15 Mo1 N2 C8 -14.7(9) . . . . ? C13 Mo1 N2 C8 179.81(17) . . . . ? C14 Mo1 N2 C8 -96.35(18) . . . . ? N1 Mo1 N2 C8 -1.48(16) . . . . ? P1 Mo1 N2 C8 88.17(17) . . . . ? C7 N1 C1 C2 -141.9(2) . . . . ? Mo1 N1 C1 C2 38.7(3) . . . . ? C7 N1 C1 C6 39.3(3) . . . . ? Mo1 N1 C1 C6 -140.11(19) . . . . ? C6 C1 C2 C3 -1.1(4) . . . . ? N1 C1 C2 C3 -179.9(2) . . . . ? C1 C2 C3 C4 2.2(4) . . . . ? C2 C3 C4 O1 177.5(2) . . . . ? C2 C3 C4 C5 -2.0(4) . . . . ? O1 C4 C5 C6 -178.9(2) . . . . ? C3 C4 C5 C6 0.6(4) . . . . ? C4 C5 C6 C1 0.5(4) . . . . ? C2 C1 C6 C5 -0.3(4) . . . . ? N1 C1 C6 C5 178.5(2) . . . . ? C1 N1 C7 C8 179.8(2) . . . . ? Mo1 N1 C7 C8 -0.7(3) . . . . ? C12 N2 C8 C9 2.0(4) . . . . ? Mo1 N2 C8 C9 -177.2(2) . . . . ? C12 N2 C8 C7 -179.1(2) . . . . ? Mo1 N2 C8 C7 1.7(3) . . . . ? N1 C7 C8 N2 -0.6(4) . . . . ? N1 C7 C8 C9 178.2(2) . . . . ? N2 C8 C9 C10 -1.0(4) . . . . ? C7 C8 C9 C10 -179.7(3) . . . . ? C8 C9 C10 C11 -0.9(5) . . . . ? C9 C10 C11 C12 1.7(5) . . . . ? C8 N2 C12 C11 -1.2(4) . . . . ? Mo1 N2 C12 C11 177.9(2) . . . . ? C10 C11 C12 N2 -0.6(5) . . . . ? C15 Mo1 C13 O13 -51(3) . . . . ? C14 Mo1 C13 O13 37(3) . . . . ? N2 Mo1 C13 O13 127(3) . . . . ? N1 Mo1 C13 O13 118(2) . . . . ? P1 Mo1 C13 O13 -143(3) . . . . ? C15 Mo1 C14 O14 77(3) . . . . ? C13 Mo1 C14 O14 -8(3) . . . . ? N2 Mo1 C14 O14 -108(3) . . . . ? N1 Mo1 C14 O14 180(100) . . . . ? P1 Mo1 C14 O14 -6(3) . . . . ? C13 Mo1 C15 O15 18(5) . . . . ? C14 Mo1 C15 O15 -66(5) . . . . ? N2 Mo1 C15 O15 -148(4) . . . . ? N1 Mo1 C15 O15 -161(5) . . . . ? P1 Mo1 C15 O15 109(5) . . . . ? C30 P1 C20 C25 -34.9(2) . . . . ? C40 P1 C20 C25 73.2(2) . . . . ? Mo1 P1 C20 C25 -156.76(19) . . . . ? C30 P1 C20 C21 149.7(2) . . . . ? C40 P1 C20 C21 -102.2(2) . . . . ? Mo1 P1 C20 C21 27.8(2) . . . . ? C25 C20 C21 C22 -1.5(4) . . . . ? P1 C20 C21 C22 174.1(2) . . . . ? C20 C21 C22 C23 0.6(4) . . . . ? C21 C22 C23 C24 0.5(5) . . . . ? C22 C23 C24 C25 -0.8(5) . . . . ? C23 C24 C25 C20 -0.1(5) . . . . ? C21 C20 C25 C24 1.2(4) . . . . ? P1 C20 C25 C24 -174.3(2) . . . . ? C20 P1 C30 C31 -48.5(2) . . . . ? C40 P1 C30 C31 -152.7(2) . . . . ? Mo1 P1 C30 C31 81.3(2) . . . . ? C20 P1 C30 C35 142.8(2) . . . . ? C40 P1 C30 C35 38.5(2) . . . . ? Mo1 P1 C30 C35 -87.4(2) . . . . ? C35 C30 C31 C32 -0.2(4) . . . . ? P1 C30 C31 C32 -169.2(2) . . . . ? C30 C31 C32 C33 0.6(5) . . . . ? C31 C32 C33 C34 -1.3(5) . . . . ? C32 C33 C34 C35 1.6(5) . . . . ? C33 C34 C35 C30 -1.2(5) . . . . ? C31 C30 C35 C34 0.5(4) . . . . ? P1 C30 C35 C34 169.3(2) . . . . ? C30 P1 C40 C41 -146.7(2) . . . . ? C20 P1 C40 C41 107.7(2) . . . . ? Mo1 P1 C40 C41 -25.3(2) . . . . ? C30 P1 C40 C45 35.7(3) . . . . ? C20 P1 C40 C45 -70.0(3) . . . . ? Mo1 P1 C40 C45 157.0(2) . . . . ? C45 C40 C41 C42 -0.2(4) . . . . ? P1 C40 C41 C42 -177.89(19) . . . . ? C40 C41 C42 C43 -0.8(4) . . . . ? C41 C42 C43 C44 1.2(4) . . . . ? C42 C43 C44 C45 -0.7(5) . . . . ? C43 C44 C45 C40 -0.2(5) . . . . ? C41 C40 C45 C44 0.7(5) . . . . ? P1 C40 C45 C44 178.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 32.07 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.726 _refine_diff_density_min -0.985 _refine_diff_density_rms 0.084 #===END #============================================================================== data_ka222 _database_code_CSD 168311 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H19 Mo N3 O4' _chemical_formula_weight 461.32 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 monoklin _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.576(2) _cell_length_b 13.114(3) _cell_length_c 13.293(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.89(3) _cell_angle_gamma 90.00 _cell_volume 2015.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type 'experimentell' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _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 'NONIUS KAPPA CCD' _diffrn_measurement_method 'O-Scan ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10509 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 30.00 _reflns_number_total 5858 _reflns_number_gt 4072 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0340P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5858 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.006 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.396252(19) 0.892084(14) 0.174244(15) 0.01664(7) Uani 1 1 d . . . O1 O -0.21040(17) 0.82909(15) 0.12601(16) 0.0354(5) Uani 1 1 d . . . O13 O 0.61654(18) 1.02819(14) 0.16911(16) 0.0392(5) Uani 1 1 d . . . O14 O 0.4745(2) 0.80380(15) -0.03156(16) 0.0487(6) Uani 1 1 d . . . O15 O 0.26024(17) 1.05934(14) 0.05176(15) 0.0355(5) Uani 1 1 d . . . N1 N 0.26393(18) 0.76978(14) 0.19601(15) 0.0206(5) Uani 1 1 d . . . N2 N 0.48637(18) 0.75902(14) 0.25148(15) 0.0212(5) Uani 1 1 d . . . N3 N 0.3046(2) 0.96422(16) 0.39596(18) 0.0334(6) Uani 1 1 d . . . C1 C 0.1418(2) 0.78231(17) 0.17635(19) 0.0206(5) Uani 1 1 d . . . C2 C 0.1013(2) 0.82573(18) 0.0864(2) 0.0239(6) Uani 1 1 d . . . C3 C -0.0166(2) 0.83955(19) 0.0669(2) 0.0244(6) Uani 1 1 d . . . C4 C -0.0937(2) 0.81340(18) 0.1389(2) 0.0249(6) Uani 1 1 d . . . C5 C -0.0531(3) 0.7717(2) 0.2296(2) 0.0296(6) Uani 1 1 d . . . C6 C 0.0642(2) 0.7551(2) 0.2478(2) 0.0267(6) Uani 1 1 d . . . C7 C 0.2997(2) 0.68582(18) 0.23739(19) 0.0225(6) Uani 1 1 d . . . C8 C 0.4214(2) 0.67369(17) 0.26329(18) 0.0218(5) Uani 1 1 d . . . C9 C 0.4707(3) 0.58251(19) 0.2965(2) 0.0288(6) Uani 1 1 d . . . C10 C 0.5875(3) 0.5774(2) 0.3191(2) 0.0314(7) Uani 1 1 d . . . C11 C 0.6531(3) 0.6648(2) 0.3106(2) 0.0286(6) Uani 1 1 d . . . C12 C 0.5994(2) 0.7533(2) 0.2760(2) 0.0256(6) Uani 1 1 d . . . C13 C 0.5327(2) 0.98024(19) 0.1720(2) 0.0261(6) Uani 1 1 d . . . C14 C 0.4449(2) 0.83619(19) 0.0432(2) 0.0267(6) Uani 1 1 d . . . C15 C 0.3115(2) 0.99629(18) 0.0990(2) 0.0243(6) Uani 1 1 d . . . C16 C 0.3408(2) 0.94382(18) 0.3188(2) 0.0265(6) Uani 1 1 d . . . C17 C 0.2567(3) 0.9771(2) 0.4963(2) 0.0369(7) Uani 1 1 d . . . C18 C 0.1616(4) 0.8950(3) 0.5051(4) 0.0590(11) Uani 1 1 d . . . C19 C 0.2040(4) 1.0855(3) 0.5049(3) 0.0564(10) Uani 1 1 d . . . C20 C 0.3562(4) 0.9619(4) 0.5741(3) 0.0669(12) Uani 1 1 d . . . H1 H -0.227(3) 0.862(2) 0.073(2) 0.045(10) Uiso 1 1 d . . . H2 H 0.156(2) 0.8476(18) 0.037(2) 0.027(7) Uiso 1 1 d . . . H3 H -0.045(3) 0.863(2) 0.009(2) 0.033(8) Uiso 1 1 d . . . H5 H -0.107(3) 0.754(2) 0.282(2) 0.039(8) Uiso 1 1 d . . . H6 H 0.090(2) 0.732(2) 0.310(2) 0.043(9) Uiso 1 1 d . . . H7 H 0.249(2) 0.6313(17) 0.2511(18) 0.019(7) Uiso 1 1 d . . . H9 H 0.425(2) 0.5330(18) 0.3012(19) 0.019(7) Uiso 1 1 d . . . H10 H 0.627(2) 0.512(2) 0.3420(19) 0.030(8) Uiso 1 1 d . . . H11 H 0.729(3) 0.664(2) 0.330(2) 0.034(8) Uiso 1 1 d . . . H12 H 0.643(2) 0.8128(18) 0.2647(19) 0.024(7) Uiso 1 1 d . . . H1A H 0.203(3) 0.837(3) 0.499(3) 0.064(12) Uiso 1 1 d . . . H1B H 0.104(3) 0.915(2) 0.454(3) 0.051(11) Uiso 1 1 d . . . H1C H 0.128(3) 0.913(2) 0.562(3) 0.057(11) Uiso 1 1 d . . . H2A H 0.135(3) 1.078(3) 0.461(3) 0.065(13) Uiso 1 1 d . . . H2B H 0.271(4) 1.130(3) 0.500(3) 0.090(15) Uiso 1 1 d . . . H2C H 0.175(2) 1.0835(18) 0.577(2) 0.024(7) Uiso 1 1 d . . . H3A H 0.393(3) 0.887(3) 0.556(3) 0.070(12) Uiso 1 1 d . . . H3B H 0.421(4) 1.029(3) 0.561(3) 0.097(14) Uiso 1 1 d . . . H3C H 0.301(5) 0.968(4) 0.639(4) 0.14(2) Uiso 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 0.01749(12) 0.01555(10) 0.01716(11) 0.00128(9) 0.00349(8) -0.00002(9) O1 0.0206(12) 0.0456(12) 0.0399(13) 0.0137(10) 0.0010(10) 0.0001(9) O13 0.0321(13) 0.0351(11) 0.0504(14) 0.0058(10) 0.0025(10) -0.0125(9) O14 0.0738(18) 0.0431(12) 0.0312(12) -0.0010(10) 0.0225(12) 0.0107(11) O15 0.0344(13) 0.0349(10) 0.0373(12) 0.0110(9) 0.0033(10) 0.0122(9) N1 0.0211(12) 0.0232(10) 0.0178(11) -0.0008(8) 0.0020(9) 0.0006(8) N2 0.0205(13) 0.0234(10) 0.0201(11) 0.0008(8) 0.0049(9) 0.0009(9) N3 0.0421(17) 0.0329(12) 0.0255(13) -0.0025(10) 0.0030(12) 0.0064(11) C1 0.0212(15) 0.0192(11) 0.0215(13) -0.0021(10) 0.0014(11) -0.0019(10) C2 0.0257(16) 0.0242(12) 0.0221(14) 0.0031(11) 0.0054(12) -0.0005(11) C3 0.0233(16) 0.0285(13) 0.0210(14) 0.0028(11) -0.0021(12) 0.0003(11) C4 0.0194(15) 0.0251(12) 0.0303(15) 0.0029(11) 0.0017(12) -0.0022(10) C5 0.0225(16) 0.0376(15) 0.0293(16) 0.0104(12) 0.0071(13) -0.0028(12) C6 0.0232(16) 0.0308(14) 0.0262(15) 0.0087(12) 0.0011(12) -0.0011(11) C7 0.0257(16) 0.0198(12) 0.0221(14) 0.0018(10) 0.0011(11) -0.0043(11) C8 0.0248(15) 0.0212(12) 0.0200(13) 0.0027(10) 0.0055(11) -0.0006(10) C9 0.0296(18) 0.0200(13) 0.0370(17) 0.0055(11) 0.0044(13) -0.0025(11) C10 0.0293(19) 0.0277(13) 0.0378(17) 0.0069(12) 0.0068(14) 0.0074(12) C11 0.0174(16) 0.0346(15) 0.0341(16) 0.0075(12) 0.0043(13) 0.0052(12) C12 0.0210(16) 0.0274(13) 0.0288(15) 0.0037(11) 0.0049(12) -0.0002(11) C13 0.0289(17) 0.0256(13) 0.0238(14) 0.0037(11) 0.0019(12) 0.0028(11) C14 0.0304(17) 0.0261(13) 0.0241(14) 0.0032(11) 0.0072(12) 0.0010(11) C15 0.0214(15) 0.0271(13) 0.0249(14) -0.0023(11) 0.0069(12) -0.0005(11) C16 0.0293(17) 0.0215(13) 0.0286(16) -0.0008(11) -0.0003(13) 0.0038(11) C17 0.049(2) 0.0392(16) 0.0238(15) -0.0008(12) 0.0107(15) 0.0004(14) C18 0.070(3) 0.053(2) 0.055(3) 0.001(2) 0.018(2) -0.010(2) C19 0.066(3) 0.052(2) 0.052(3) 0.0069(18) 0.014(2) 0.009(2) C20 0.077(3) 0.086(3) 0.038(2) 0.003(2) -0.001(2) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C15 1.931(3) . ? Mo1 C13 1.958(3) . ? Mo1 C14 1.997(3) . ? Mo1 C16 2.166(3) . ? Mo1 N1 2.247(2) . ? Mo1 N2 2.254(2) . ? O1 C4 1.369(3) . ? O1 H1 0.84(3) . ? O13 C13 1.159(3) . ? O14 C14 1.148(3) . ? O15 C15 1.180(3) . ? N1 C7 1.290(3) . ? N1 C1 1.434(3) . ? N2 C12 1.334(3) . ? N2 C8 1.362(3) . ? N3 C16 1.159(3) . ? N3 C17 1.480(3) . ? C1 C2 1.385(3) . ? C1 C6 1.386(4) . ? C2 C3 1.387(4) . ? C2 H2 0.98(3) . ? C3 C4 1.385(4) . ? C3 H3 0.88(3) . ? C4 C5 1.384(4) . ? C5 C6 1.385(4) . ? C5 H5 0.99(3) . ? C6 H6 0.92(3) . ? C7 C8 1.443(4) . ? C7 H7 0.95(2) . ? C8 C9 1.387(3) . ? C9 C10 1.372(4) . ? C9 H9 0.85(2) . ? C10 C11 1.383(4) . ? C10 H10 1.01(3) . ? C11 C12 1.384(4) . ? C11 H11 0.90(3) . ? C12 H12 0.94(2) . ? C17 C20 1.522(5) . ? C17 C18 1.548(5) . ? C17 C19 1.554(5) . ? C18 H1A 0.90(4) . ? C18 H1B 0.96(3) . ? C18 H1C 0.90(3) . ? C19 H2A 0.97(4) . ? C19 H2B 0.98(4) . ? C19 H2C 1.04(3) . ? C20 H3A 1.10(3) . ? C20 H3B 1.17(4) . ? C20 H3C 1.10(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 C15 Mo1 C13 87.91(11) . . ? C15 Mo1 C14 88.07(11) . . ? C13 Mo1 C14 86.59(11) . . ? C15 Mo1 C16 94.14(10) . . ? C13 Mo1 C16 95.95(11) . . ? C14 Mo1 C16 176.69(9) . . ? C15 Mo1 N1 103.88(9) . . ? C13 Mo1 N1 168.20(9) . . ? C14 Mo1 N1 94.27(9) . . ? C16 Mo1 N1 82.82(9) . . ? C15 Mo1 N2 174.25(9) . . ? C13 Mo1 N2 96.25(9) . . ? C14 Mo1 N2 88.22(9) . . ? C16 Mo1 N2 89.39(8) . . ? N1 Mo1 N2 72.03(8) . . ? C4 O1 H1 111(2) . . ? C7 N1 C1 117.9(2) . . ? C7 N1 Mo1 117.29(18) . . ? C1 N1 Mo1 124.54(14) . . ? C12 N2 C8 117.8(2) . . ? C12 N2 Mo1 125.50(16) . . ? C8 N2 Mo1 116.30(17) . . ? C16 N3 C17 173.2(3) . . ? C2 C1 C6 119.6(3) . . ? C2 C1 N1 119.5(2) . . ? C6 C1 N1 120.8(2) . . ? C1 C2 C3 120.1(3) . . ? C1 C2 H2 119.8(16) . . ? C3 C2 H2 120.1(16) . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3 118(2) . . ? C2 C3 H3 122(2) . . ? O1 C4 C5 117.3(2) . . ? O1 C4 C3 122.9(2) . . ? C5 C4 C3 119.8(3) . . ? C4 C5 C6 120.1(3) . . ? C4 C5 H5 120.6(17) . . ? C6 C5 H5 119.4(17) . . ? C5 C6 C1 120.2(3) . . ? C5 C6 H6 118.8(18) . . ? C1 C6 H6 120.7(18) . . ? N1 C7 C8 119.0(2) . . ? N1 C7 H7 122.6(15) . . ? C8 C7 H7 118.4(15) . . ? N2 C8 C9 121.6(2) . . ? N2 C8 C7 114.9(2) . . ? C9 C8 C7 123.5(2) . . ? C10 C9 C8 119.8(3) . . ? C10 C9 H9 124.4(18) . . ? C8 C9 H9 115.8(18) . . ? C9 C10 C11 118.7(3) . . ? C9 C10 H10 121.9(15) . . ? C11 C10 H10 119.3(15) . . ? C10 C11 C12 118.9(3) . . ? C10 C11 H11 119.8(17) . . ? C12 C11 H11 121.3(18) . . ? N2 C12 C11 123.2(3) . . ? N2 C12 H12 115.9(16) . . ? C11 C12 H12 120.8(16) . . ? O13 C13 Mo1 176.5(2) . . ? O14 C14 Mo1 179.0(3) . . ? O15 C15 Mo1 179.0(2) . . ? N3 C16 Mo1 174.0(2) . . ? N3 C17 C20 107.0(3) . . ? N3 C17 C18 106.8(3) . . ? C20 C17 C18 112.0(3) . . ? N3 C17 C19 109.7(3) . . ? C20 C17 C19 110.9(3) . . ? C18 C17 C19 110.3(3) . . ? C17 C18 H1A 101(2) . . ? C17 C18 H1B 103(2) . . ? H1A C18 H1B 122(3) . . ? C17 C18 H1C 102(2) . . ? H1A C18 H1C 123(3) . . ? H1B C18 H1C 102(3) . . ? C17 C19 H2A 100(2) . . ? C17 C19 H2B 103(3) . . ? H2A C19 H2B 131(3) . . ? C17 C19 H2C 101.1(14) . . ? H2A C19 H2C 104(3) . . ? H2B C19 H2C 112(3) . . ? C17 C20 H3A 105(2) . . ? C17 C20 H3B 105(2) . . ? H3A C20 H3B 112(3) . . ? C17 C20 H3C 94(3) . . ? H3A C20 H3C 119(3) . . ? H3B C20 H3C 118(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 Mo1 N1 C7 174.29(19) . . . . ? C13 Mo1 N1 C7 -8.5(5) . . . . ? C14 Mo1 N1 C7 85.23(19) . . . . ? C16 Mo1 N1 C7 -93.20(19) . . . . ? N2 Mo1 N1 C7 -1.50(18) . . . . ? C15 Mo1 N1 C1 -12.1(2) . . . . ? C13 Mo1 N1 C1 165.1(4) . . . . ? C14 Mo1 N1 C1 -101.21(19) . . . . ? C16 Mo1 N1 C1 80.37(19) . . . . ? N2 Mo1 N1 C1 172.1(2) . . . . ? C15 Mo1 N2 C12 132.3(9) . . . . ? C13 Mo1 N2 C12 -3.8(2) . . . . ? C14 Mo1 N2 C12 82.5(2) . . . . ? C16 Mo1 N2 C12 -99.8(2) . . . . ? N1 Mo1 N2 C12 177.6(2) . . . . ? C15 Mo1 N2 C8 -39.9(10) . . . . ? C13 Mo1 N2 C8 -176.02(18) . . . . ? C14 Mo1 N2 C8 -89.65(18) . . . . ? C16 Mo1 N2 C8 88.07(18) . . . . ? N1 Mo1 N2 C8 5.42(16) . . . . ? C7 N1 C1 C2 -138.5(2) . . . . ? Mo1 N1 C1 C2 47.9(3) . . . . ? C7 N1 C1 C6 43.9(3) . . . . ? Mo1 N1 C1 C6 -129.6(2) . . . . ? C6 C1 C2 C3 -1.6(4) . . . . ? N1 C1 C2 C3 -179.1(2) . . . . ? C1 C2 C3 C4 2.4(4) . . . . ? C2 C3 C4 O1 177.2(2) . . . . ? C2 C3 C4 C5 -1.2(4) . . . . ? O1 C4 C5 C6 -179.2(2) . . . . ? C3 C4 C5 C6 -0.8(4) . . . . ? C4 C5 C6 C1 1.6(4) . . . . ? C2 C1 C6 C5 -0.4(4) . . . . ? N1 C1 C6 C5 177.2(2) . . . . ? C1 N1 C7 C8 -176.5(2) . . . . ? Mo1 N1 C7 C8 -2.4(3) . . . . ? C12 N2 C8 C9 -2.1(4) . . . . ? Mo1 N2 C8 C9 170.7(2) . . . . ? C12 N2 C8 C7 178.8(2) . . . . ? Mo1 N2 C8 C7 -8.4(3) . . . . ? N1 C7 C8 N2 7.3(3) . . . . ? N1 C7 C8 C9 -171.8(2) . . . . ? N2 C8 C9 C10 0.6(4) . . . . ? C7 C8 C9 C10 179.7(3) . . . . ? C8 C9 C10 C11 1.6(4) . . . . ? C9 C10 C11 C12 -2.3(4) . . . . ? C8 N2 C12 C11 1.3(4) . . . . ? Mo1 N2 C12 C11 -170.7(2) . . . . ? C10 C11 C12 N2 0.9(4) . . . . ? C15 Mo1 C13 O13 -131(4) . . . . ? C14 Mo1 C13 O13 -43(4) . . . . ? C16 Mo1 C13 O13 135(4) . . . . ? N1 Mo1 C13 O13 52(4) . . . . ? N2 Mo1 C13 O13 45(4) . . . . ? C15 Mo1 C14 O14 139(13) . . . . ? C13 Mo1 C14 O14 51(13) . . . . ? C16 Mo1 C14 O14 -89(13) . . . . ? N1 Mo1 C14 O14 -117(13) . . . . ? N2 Mo1 C14 O14 -45(13) . . . . ? C13 Mo1 C15 O15 86(14) . . . . ? C14 Mo1 C15 O15 0(14) . . . . ? C16 Mo1 C15 O15 -178(100) . . . . ? N1 Mo1 C15 O15 -94(14) . . . . ? N2 Mo1 C15 O15 -50(14) . . . . ? C17 N3 C16 Mo1 33(4) . . . . ? C15 Mo1 C16 N3 104(2) . . . . ? C13 Mo1 C16 N3 -167(2) . . . . ? C14 Mo1 C16 N3 -28(4) . . . . ? N1 Mo1 C16 N3 1(2) . . . . ? N2 Mo1 C16 N3 -71(2) . . . . ? C16 N3 C17 C20 83(2) . . . . ? C16 N3 C17 C18 -38(3) . . . . ? C16 N3 C17 C19 -157(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.762 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.104 #===END #============================================================================== data_ka349 _database_code_CSD 168312 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H21 Mo N3 O4' _chemical_formula_weight 487.36 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 monoklin _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.537(2) _cell_length_b 12.954(3) _cell_length_c 14.109(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.72(3) _cell_angle_gamma 90.00 _cell_volume 2094.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.660 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _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 'NONIUS KAPPA CCD' _diffrn_measurement_method 'O-Scan ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19800 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 37.02 _reflns_number_total 10629 _reflns_number_gt 8333 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0501P)^2^+0.4885P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10629 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.1005 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.077 _refine_ls_shift/su_mean 0.006 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 0.894435(9) 0.864354(9) 0.154978(8) 0.01875(4) Uani 1 1 d . . . O1 O 0.27865(10) 0.80896(11) 0.10136(10) 0.0349(3) Uani 1 1 d . . . O13 O 1.11392(12) 1.00434(11) 0.15254(11) 0.0443(3) Uani 1 1 d . . . O14 O 0.94982(16) 0.79084(12) -0.04800(10) 0.0509(4) Uani 1 1 d . . . O15 O 0.75586(11) 1.04658(10) 0.05182(9) 0.0364(3) Uani 1 1 d . . . N1 N 0.75824(10) 0.74482(9) 0.18198(8) 0.0215(2) Uani 1 1 d . . . N2 N 0.98726(10) 0.72993(9) 0.23164(8) 0.0203(2) Uani 1 1 d . . . N3 N 0.83782(15) 0.92476(12) 0.37217(11) 0.0375(3) Uani 1 1 d . . . C1 C 0.63527(12) 0.75876(11) 0.16142(10) 0.0219(2) Uani 1 1 d . . . C2 C 0.59132(13) 0.80340(11) 0.07458(10) 0.0234(2) Uani 1 1 d . . . C3 C 0.47224(13) 0.81884(12) 0.05215(10) 0.0246(3) Uani 1 1 d . . . C4 C 0.39603(12) 0.79229(12) 0.11774(11) 0.0252(3) Uani 1 1 d . . . C5 C 0.43970(14) 0.74901(15) 0.20481(12) 0.0322(3) Uani 1 1 d . . . C6 C 0.55803(14) 0.73168(14) 0.22638(11) 0.0292(3) Uani 1 1 d . . . C7 C 0.79513(13) 0.66370(12) 0.22982(10) 0.0239(2) Uani 1 1 d . . . C8 C 0.91957(13) 0.65119(11) 0.25740(10) 0.0218(2) Uani 1 1 d . . . C9 C 0.96611(14) 0.56541(12) 0.30808(11) 0.0265(3) Uani 1 1 d . . . C10 C 1.08571(14) 0.56208(13) 0.33603(11) 0.0289(3) Uani 1 1 d . . . C11 C 1.15468(14) 0.64279(12) 0.31098(12) 0.0276(3) Uani 1 1 d . . . C12 C 1.10261(12) 0.72401(11) 0.25775(10) 0.0238(2) Uani 1 1 d . . . C13 C 1.03158(13) 0.95332(12) 0.15353(11) 0.0262(3) Uani 1 1 d . . . C14 C 0.92756(15) 0.81529(12) 0.02625(11) 0.0289(3) Uani 1 1 d . . . C15 C 0.80643(13) 0.97654(12) 0.09087(10) 0.0244(3) Uani 1 1 d . . . C16 C 0.86071(14) 0.91110(12) 0.29544(11) 0.0283(3) Uani 1 1 d . . . C17 C 0.8029(2) 0.93921(14) 0.46633(12) 0.0398(4) Uani 1 1 d . . . C18 C 0.6754(2) 0.9148(2) 0.46439(19) 0.0614(7) Uani 1 1 d . . . H18A H 0.6607 0.8438 0.4446 0.108(4) Uiso 1 1 calc R . . H18B H 0.6297 0.9596 0.4194 0.108(4) Uiso 1 1 calc R . . C19 C 0.6409(4) 0.9314(3) 0.5653(2) 0.0996(14) Uani 1 1 d . . . H19A H 0.5580 0.9181 0.5647 0.108(4) Uiso 1 1 calc R . . H19B H 0.6828 0.8824 0.6087 0.108(4) Uiso 1 1 calc R . . C20 C 0.6668(6) 1.0370(3) 0.6003(3) 0.153(3) Uani 1 1 d . . . H20A H 0.6183 1.0854 0.5611 0.108(4) Uiso 1 1 calc R . . H20B H 0.6475 1.0428 0.6652 0.108(4) Uiso 1 1 calc R . . C21 C 0.7882(6) 1.0637(3) 0.5983(2) 0.142(3) Uani 1 1 d . . . H21A H 0.8354 1.0220 0.6452 0.108(4) Uiso 1 1 calc R . . H21B H 0.7993 1.1354 0.6170 0.108(4) Uiso 1 1 calc R . . C22 C 0.8326(4) 1.0481(2) 0.49980(18) 0.0757(10) Uani 1 1 d . . . H22A H 0.7957 1.0976 0.4542 0.108(4) Uiso 1 1 calc R . . H22B H 0.9164 1.0587 0.5052 0.108(4) Uiso 1 1 calc R . . H1 H 0.261(3) 0.841(2) 0.061(2) 0.069(10) Uiso 1 1 d . . . H2 H 0.6468(19) 0.8219(17) 0.0300(15) 0.032(5) Uiso 1 1 d . . . H3 H 0.440(2) 0.8443(19) -0.0034(17) 0.040(6) Uiso 1 1 d . . . H5 H 0.385(2) 0.734(2) 0.2454(18) 0.054(7) Uiso 1 1 d . . . H6 H 0.5886(19) 0.7131(17) 0.2855(16) 0.037(6) Uiso 1 1 d . . . H7 H 0.7402(18) 0.6119(15) 0.2494(14) 0.030(6) Uiso 1 1 d . . . H9 H 0.918(2) 0.5111(19) 0.3250(16) 0.043(6) Uiso 1 1 d . . . H10 H 1.1167(17) 0.5052(17) 0.3662(14) 0.028(5) Uiso 1 1 d . . . H11 H 1.233(2) 0.6440(15) 0.3320(16) 0.033(6) Uiso 1 1 d . . . H12 H 1.1488(16) 0.7759(14) 0.2374(13) 0.018(4) Uiso 1 1 d . . . H17 H 0.858(2) 0.894(2) 0.5129(18) 0.053(7) Uiso 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 0.01846(6) 0.01838(6) 0.01944(6) 0.00277(4) 0.00235(4) 0.00052(4) O1 0.0186(5) 0.0395(7) 0.0464(7) 0.0154(6) 0.0025(5) 0.0018(4) O13 0.0335(7) 0.0393(7) 0.0585(8) 0.0100(6) -0.0009(6) -0.0142(5) O14 0.0845(12) 0.0418(8) 0.0289(6) -0.0011(6) 0.0172(7) 0.0099(8) O15 0.0349(6) 0.0346(6) 0.0400(6) 0.0129(5) 0.0055(5) 0.0120(5) N1 0.0201(5) 0.0222(5) 0.0220(5) 0.0025(4) 0.0019(4) -0.0006(4) N2 0.0204(5) 0.0196(5) 0.0209(5) 0.0018(4) 0.0027(4) 0.0009(4) N3 0.0507(9) 0.0336(7) 0.0293(6) -0.0004(6) 0.0097(6) 0.0003(6) C1 0.0197(6) 0.0232(6) 0.0225(5) 0.0019(5) 0.0016(4) -0.0015(4) C2 0.0219(6) 0.0261(6) 0.0224(6) 0.0032(5) 0.0030(5) 0.0009(5) C3 0.0226(6) 0.0263(7) 0.0245(6) 0.0041(5) 0.0006(5) 0.0007(5) C4 0.0185(6) 0.0242(6) 0.0327(7) 0.0031(5) 0.0018(5) -0.0009(5) C5 0.0244(7) 0.0404(9) 0.0329(7) 0.0121(7) 0.0077(6) -0.0003(6) C6 0.0241(7) 0.0379(8) 0.0257(6) 0.0090(6) 0.0030(5) -0.0003(6) C7 0.0225(6) 0.0225(6) 0.0260(6) 0.0043(5) 0.0006(5) -0.0018(5) C8 0.0222(6) 0.0204(6) 0.0225(6) 0.0023(4) 0.0013(5) 0.0008(4) C9 0.0280(7) 0.0218(6) 0.0297(7) 0.0058(5) 0.0033(5) 0.0009(5) C10 0.0297(7) 0.0245(6) 0.0322(7) 0.0059(5) 0.0021(6) 0.0069(5) C11 0.0225(7) 0.0287(7) 0.0311(7) 0.0041(5) 0.0006(5) 0.0052(5) C12 0.0212(6) 0.0239(6) 0.0264(6) 0.0022(5) 0.0032(5) 0.0015(5) C13 0.0250(6) 0.0240(6) 0.0292(6) 0.0045(5) 0.0008(5) -0.0007(5) C14 0.0354(8) 0.0244(7) 0.0267(6) 0.0023(5) 0.0031(5) 0.0024(6) C15 0.0225(6) 0.0260(6) 0.0250(6) 0.0035(5) 0.0040(5) 0.0017(5) C16 0.0318(7) 0.0246(7) 0.0284(7) 0.0022(5) 0.0037(5) 0.0016(5) C17 0.0683(13) 0.0294(8) 0.0232(7) 0.0008(6) 0.0122(7) 0.0040(8) C18 0.0728(17) 0.0591(15) 0.0593(14) 0.0058(12) 0.0378(13) -0.0024(13) C19 0.154(4) 0.078(2) 0.085(2) 0.0305(18) 0.090(2) 0.037(2) C20 0.331(8) 0.063(2) 0.094(3) 0.0405(19) 0.145(4) 0.088(3) C21 0.340(8) 0.0534(18) 0.0335(13) -0.0207(13) 0.030(3) -0.023(3) C22 0.142(3) 0.0466(13) 0.0379(11) -0.0105(10) 0.0073(14) -0.0253(16) _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 C15 1.9354(15) . ? Mo1 C13 1.9594(15) . ? Mo1 C14 2.0028(17) . ? Mo1 C16 2.1508(16) . ? Mo1 N2 2.2534(12) . ? Mo1 N1 2.2698(12) . ? O1 C4 1.3641(18) . ? O1 H1 0.72(3) . ? O13 C13 1.1587(19) . ? O14 C14 1.152(2) . ? O15 C15 1.1799(18) . ? N1 C7 1.2938(19) . ? N1 C1 1.4259(18) . ? N2 C12 1.3408(18) . ? N2 C8 1.3597(18) . ? N3 C16 1.157(2) . ? N3 C17 1.445(2) . ? C1 C2 1.3955(19) . ? C1 C6 1.396(2) . ? C2 C3 1.388(2) . ? C2 H2 0.98(2) . ? C3 C4 1.392(2) . ? C3 H3 0.89(2) . ? C4 C5 1.390(2) . ? C5 C6 1.382(2) . ? C5 H5 0.92(3) . ? C6 H6 0.90(2) . ? C7 C8 1.452(2) . ? C7 H7 0.99(2) . ? C8 C9 1.395(2) . ? C9 C10 1.391(2) . ? C9 H9 0.94(2) . ? C10 C11 1.385(2) . ? C10 H10 0.90(2) . ? C11 C12 1.388(2) . ? C11 H11 0.91(2) . ? C12 H12 0.924(18) . ? C17 C18 1.501(3) . ? C17 C22 1.515(3) . ? C17 H17 1.04(3) . ? C18 C19 1.539(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.473(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.446(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.550(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? 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 C15 Mo1 C13 86.19(6) . . ? C15 Mo1 C14 87.69(6) . . ? C13 Mo1 C14 86.40(7) . . ? C15 Mo1 C16 94.45(6) . . ? C13 Mo1 C16 94.43(7) . . ? C14 Mo1 C16 177.74(6) . . ? C15 Mo1 N2 176.75(5) . . ? C13 Mo1 N2 96.92(6) . . ? C14 Mo1 N2 93.42(6) . . ? C16 Mo1 N2 84.40(5) . . ? C15 Mo1 N1 104.78(6) . . ? C13 Mo1 N1 168.14(5) . . ? C14 Mo1 N1 98.34(6) . . ? C16 Mo1 N1 80.45(6) . . ? N2 Mo1 N1 72.05(5) . . ? C4 O1 H1 114(3) . . ? C7 N1 C1 117.90(12) . . ? C7 N1 Mo1 116.72(10) . . ? C1 N1 Mo1 124.84(9) . . ? C12 N2 C8 117.79(12) . . ? C12 N2 Mo1 125.22(10) . . ? C8 N2 Mo1 116.89(9) . . ? C16 N3 C17 176.8(2) . . ? C2 C1 C6 119.11(13) . . ? C2 C1 N1 118.80(13) . . ? C6 C1 N1 122.07(13) . . ? C3 C2 C1 120.55(14) . . ? C3 C2 H2 121.5(12) . . ? C1 C2 H2 117.9(12) . . ? C2 C3 C4 119.88(13) . . ? C2 C3 H3 123.3(16) . . ? C4 C3 H3 116.8(16) . . ? O1 C4 C5 117.61(14) . . ? O1 C4 C3 122.68(14) . . ? C5 C4 C3 119.69(14) . . ? C6 C5 C4 120.44(15) . . ? C6 C5 H5 124.1(16) . . ? C4 C5 H5 115.5(16) . . ? C5 C6 C1 120.31(14) . . ? C5 C6 H6 121.2(14) . . ? C1 C6 H6 117.7(14) . . ? N1 C7 C8 119.02(13) . . ? N1 C7 H7 121.1(12) . . ? C8 C7 H7 119.8(12) . . ? N2 C8 C9 122.41(13) . . ? N2 C8 C7 115.19(12) . . ? C9 C8 C7 122.39(13) . . ? C10 C9 C8 118.68(14) . . ? C10 C9 H9 119.8(14) . . ? C8 C9 H9 121.4(14) . . ? C11 C10 C9 119.01(14) . . ? C11 C10 H10 121.9(13) . . ? C9 C10 H10 119.0(13) . . ? C10 C11 C12 119.03(15) . . ? C10 C11 H11 120.2(13) . . ? C12 C11 H11 120.7(13) . . ? N2 C12 C11 123.01(14) . . ? N2 C12 H12 117.6(11) . . ? C11 C12 H12 119.4(11) . . ? O13 C13 Mo1 178.76(15) . . ? O14 C14 Mo1 176.93(16) . . ? O15 C15 Mo1 177.99(13) . . ? N3 C16 Mo1 172.07(15) . . ? N3 C17 C18 109.51(17) . . ? N3 C17 C22 109.26(18) . . ? C18 C17 C22 112.8(2) . . ? N3 C17 H17 107.1(15) . . ? C18 C17 H17 114.7(15) . . ? C22 C17 H17 103.1(15) . . ? C17 C18 C19 108.2(3) . . ? C17 C18 H18A 110.0 . . ? C19 C18 H18A 110.0 . . ? C17 C18 H18B 110.1 . . ? C19 C18 H18B 110.0 . . ? H18A C18 H18B 108.4 . . ? C20 C19 C18 112.1(2) . . ? C20 C19 H19A 109.2 . . ? C18 C19 H19A 109.2 . . ? C20 C19 H19B 109.2 . . ? C18 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C21 C20 C19 112.0(3) . . ? C21 C20 H20A 109.2 . . ? C19 C20 H20A 109.2 . . ? C21 C20 H20B 109.2 . . ? C19 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C20 C21 C22 114.1(3) . . ? C20 C21 H21A 108.7 . . ? C22 C21 H21A 108.7 . . ? C20 C21 H21B 108.7 . . ? C22 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C17 C22 C21 108.3(2) . . ? C17 C22 H22A 110.0 . . ? C21 C22 H22A 110.0 . . ? C17 C22 H22B 110.0 . . ? C21 C22 H22B 110.0 . . ? H22A C22 H22B 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 Mo1 N1 C7 -176.03(11) . . . . ? C13 Mo1 N1 C7 -18.7(3) . . . . ? C14 Mo1 N1 C7 94.16(12) . . . . ? C16 Mo1 N1 C7 -83.91(12) . . . . ? N2 Mo1 N1 C7 3.25(11) . . . . ? C15 Mo1 N1 C1 -4.70(12) . . . . ? C13 Mo1 N1 C1 152.6(3) . . . . ? C14 Mo1 N1 C1 -94.51(12) . . . . ? C16 Mo1 N1 C1 87.42(12) . . . . ? N2 Mo1 N1 C1 174.58(12) . . . . ? C15 Mo1 N2 C12 -166.5(9) . . . . ? C13 Mo1 N2 C12 -3.26(12) . . . . ? C14 Mo1 N2 C12 83.53(12) . . . . ? C16 Mo1 N2 C12 -97.06(12) . . . . ? N1 Mo1 N2 C12 -178.81(12) . . . . ? C15 Mo1 N2 C8 10.1(10) . . . . ? C13 Mo1 N2 C8 173.27(10) . . . . ? C14 Mo1 N2 C8 -99.95(11) . . . . ? C16 Mo1 N2 C8 79.46(11) . . . . ? N1 Mo1 N2 C8 -2.29(10) . . . . ? C7 N1 C1 C2 -144.80(15) . . . . ? Mo1 N1 C1 C2 43.96(17) . . . . ? C7 N1 C1 C6 36.9(2) . . . . ? Mo1 N1 C1 C6 -134.33(13) . . . . ? C6 C1 C2 C3 -1.3(2) . . . . ? N1 C1 C2 C3 -179.63(14) . . . . ? C1 C2 C3 C4 1.8(2) . . . . ? C2 C3 C4 O1 177.59(15) . . . . ? C2 C3 C4 C5 -1.0(2) . . . . ? O1 C4 C5 C6 -178.98(17) . . . . ? C3 C4 C5 C6 -0.4(3) . . . . ? C4 C5 C6 C1 0.9(3) . . . . ? C2 C1 C6 C5 0.0(3) . . . . ? N1 C1 C6 C5 178.24(16) . . . . ? C1 N1 C7 C8 -175.80(13) . . . . ? Mo1 N1 C7 C8 -3.85(18) . . . . ? C12 N2 C8 C9 -0.9(2) . . . . ? Mo1 N2 C8 C9 -177.71(11) . . . . ? C12 N2 C8 C7 178.04(13) . . . . ? Mo1 N2 C8 C7 1.25(16) . . . . ? N1 C7 C8 N2 1.8(2) . . . . ? N1 C7 C8 C9 -179.29(14) . . . . ? N2 C8 C9 C10 2.2(2) . . . . ? C7 C8 C9 C10 -176.65(15) . . . . ? C8 C9 C10 C11 -1.3(2) . . . . ? C9 C10 C11 C12 -0.8(2) . . . . ? C8 N2 C12 C11 -1.3(2) . . . . ? Mo1 N2 C12 C11 175.17(11) . . . . ? C10 C11 C12 N2 2.2(2) . . . . ? C15 Mo1 C13 O13 -148(7) . . . . ? C14 Mo1 C13 O13 -60(7) . . . . ? C16 Mo1 C13 O13 118(7) . . . . ? N2 Mo1 C13 O13 33(7) . . . . ? N1 Mo1 C13 O13 54(7) . . . . ? C15 Mo1 C14 O14 71(3) . . . . ? C13 Mo1 C14 O14 -16(3) . . . . ? C16 Mo1 C14 O14 -128(3) . . . . ? N2 Mo1 C14 O14 -113(3) . . . . ? N1 Mo1 C14 O14 175(3) . . . . ? C13 Mo1 C15 O15 1(4) . . . . ? C14 Mo1 C15 O15 -85(4) . . . . ? C16 Mo1 C15 O15 95(4) . . . . ? N2 Mo1 C15 O15 165(3) . . . . ? N1 Mo1 C15 O15 177(100) . . . . ? C17 N3 C16 Mo1 -48(4) . . . . ? C15 Mo1 C16 N3 125.9(11) . . . . ? C13 Mo1 C16 N3 -147.5(11) . . . . ? C14 Mo1 C16 N3 -36(2) . . . . ? N2 Mo1 C16 N3 -51.0(11) . . . . ? N1 Mo1 C16 N3 21.7(11) . . . . ? C16 N3 C17 C18 -9(3) . . . . ? C16 N3 C17 C22 -133(3) . . . . ? N3 C17 C18 C19 -179.7(2) . . . . ? C22 C17 C18 C19 -57.8(3) . . . . ? C17 C18 C19 C20 57.0(4) . . . . ? C18 C19 C20 C21 -55.9(5) . . . . ? C19 C20 C21 C22 53.9(5) . . . . ? N3 C17 C22 C21 176.9(3) . . . . ? C18 C17 C22 C21 54.8(4) . . . . ? C20 C21 C22 C17 -52.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 37.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.669 _refine_diff_density_min -1.297 _refine_diff_density_rms 0.090 #===END