Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Heinze, Katja' 'Jacob, Volker' _publ_contact_author_name 'Dr Katja Heinze' _publ_contact_author_address ; Inorganic Chemistry University of Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg GERMANY ; _publ_contact_author_email 'KATJA.HEINZE@URZ.UNI-HEIDELBERG.DE' _publ_section_title ; Hydrogen bonds in crystals of HO-(N-N')M(CO)3L complexes: chains, dimers and an unexpected hexamer ; 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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.0560(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 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_ka384 _database_code_CSD 179589 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H10 Cr N2 O5' _chemical_formula_weight 362.26 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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 35.203(5) _cell_length_b 35.203(5) _cell_length_c 6.5260(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7004(2) _cell_formula_units_Z 18 _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 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3312 _exptl_absorpt_coefficient_mu 0.764 _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 46190 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3566 _reflns_number_gt 2471 _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^)+(0.0396P)^2^+13.5916P] 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 3566 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.335 _refine_ls_shift/su_mean 0.009 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.649787(13) 0.101922(13) 0.62225(6) 0.02113(13) Uani 1 1 d . . . O1 O 0.66116(8) 0.25956(7) -0.0980(4) 0.0489(7) Uani 1 1 d . . . H1 H 0.6807 0.2698 -0.1844 0.065(14) Uiso 1 1 calc R . . O13 O 0.59306(7) 0.02068(7) 0.8688(3) 0.0384(5) Uani 1 1 d . . . O14 O 0.60646(6) 0.13684(7) 0.9086(3) 0.0355(5) Uani 1 1 d . . . O15 O 0.57059(6) 0.07843(6) 0.3630(3) 0.0364(5) Uani 1 1 d . . . O16 O 0.66424(7) 0.04100(7) 0.3390(3) 0.0378(5) Uani 1 1 d . . . N1 N 0.69395(7) 0.16194(7) 0.4779(3) 0.0209(5) Uani 1 1 d . . . N2 N 0.70973(7) 0.12229(7) 0.7753(3) 0.0224(5) Uani 1 1 d . . . C1 C 0.68471(8) 0.18515(8) 0.3220(4) 0.0216(6) Uani 1 1 d . . . C2 C 0.64990(9) 0.19286(9) 0.3501(4) 0.0249(6) Uani 1 1 d . . . H2 H 0.6315 0.1810 0.4629 0.025(2) Uiso 1 1 calc R . . C3 C 0.64253(9) 0.21818(9) 0.2105(5) 0.0284(6) Uani 1 1 d . . . H3 H 0.6198 0.2240 0.2314 0.025(2) Uiso 1 1 calc R . . C4 C 0.66927(9) 0.23475(9) 0.0399(5) 0.0303(7) Uani 1 1 d . . . C5 C 0.70319(9) 0.22609(9) 0.0072(4) 0.0272(6) Uani 1 1 d . . . H5 H 0.7207 0.2369 -0.1092 0.025(2) Uiso 1 1 calc R . . C6 C 0.71092(8) 0.20138(8) 0.1483(4) 0.0237(6) Uani 1 1 d . . . H6 H 0.7337 0.1956 0.1270 0.025(2) Uiso 1 1 calc R . . C7 C 0.73436(8) 0.18003(9) 0.5367(4) 0.0227(6) Uani 1 1 d . . . H7 H 0.7559 0.2059 0.4769 0.025(2) Uiso 1 1 calc R . . C8 C 0.74516(9) 0.15882(8) 0.6984(4) 0.0227(6) Uani 1 1 d . . . C9 C 0.78744(9) 0.17481(9) 0.7712(4) 0.0255(6) Uani 1 1 d . . . H9 H 0.8108 0.1994 0.7120 0.025(2) Uiso 1 1 calc R . . C10 C 0.79427(9) 0.15367(9) 0.9324(4) 0.0298(6) Uani 1 1 d . . . H10 H 0.8223 0.1637 0.9841 0.025(2) Uiso 1 1 calc R . . C11 C 0.75853(9) 0.11731(9) 1.0156(4) 0.0308(7) Uani 1 1 d . . . H11 H 0.7622 0.1030 1.1271 0.025(2) Uiso 1 1 calc R . . C12 C 0.71709(9) 0.10213(9) 0.9327(4) 0.0277(6) Uani 1 1 d . . . H12 H 0.6935 0.0771 0.9880 0.025(2) Uiso 1 1 calc R . . C13 C 0.61623(9) 0.05189(9) 0.7749(4) 0.0253(6) Uani 1 1 d . . . C14 C 0.62653(9) 0.12693(9) 0.8027(4) 0.0260(6) Uani 1 1 d . . . C15 C 0.60215(9) 0.08850(8) 0.4603(4) 0.0253(6) Uani 1 1 d . . . C16 C 0.66155(9) 0.06582(9) 0.4430(4) 0.0255(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0204(2) 0.0208(2) 0.0208(2) 0.00143(18) 0.00059(18) 0.00936(19) O1 0.0365(13) 0.0346(13) 0.0633(17) 0.0231(12) -0.0167(13) 0.0085(11) O13 0.0414(13) 0.0294(11) 0.0380(13) 0.0099(10) 0.0105(10) 0.0128(10) O14 0.0289(11) 0.0354(12) 0.0383(13) -0.0084(10) 0.0057(9) 0.0130(10) O15 0.0308(11) 0.0312(11) 0.0469(14) -0.0012(10) -0.0140(10) 0.0152(9) O16 0.0457(13) 0.0357(12) 0.0322(12) -0.0052(10) 0.0078(10) 0.0204(11) N1 0.0216(11) 0.0217(11) 0.0213(12) 0.0001(9) 0.0008(9) 0.0122(10) N2 0.0264(12) 0.0231(12) 0.0199(11) -0.0003(9) 0.0011(9) 0.0140(10) C1 0.0202(13) 0.0174(13) 0.0245(14) -0.0019(11) -0.0030(11) 0.0075(11) C2 0.0221(14) 0.0223(14) 0.0285(15) 0.0016(11) 0.0028(11) 0.0097(12) C3 0.0197(14) 0.0240(14) 0.0430(18) 0.0012(13) -0.0035(13) 0.0120(12) C4 0.0230(14) 0.0199(14) 0.0421(18) 0.0069(12) -0.0110(13) 0.0064(12) C5 0.0225(14) 0.0251(14) 0.0264(15) 0.0051(12) -0.0016(11) 0.0063(12) C6 0.0210(13) 0.0243(14) 0.0265(15) -0.0019(11) -0.0036(11) 0.0119(12) C7 0.0210(14) 0.0227(14) 0.0213(14) 0.0002(11) 0.0021(11) 0.0087(11) C8 0.0250(14) 0.0224(14) 0.0214(14) -0.0009(11) -0.0004(11) 0.0122(12) C9 0.0256(14) 0.0258(15) 0.0254(15) -0.0018(11) -0.0016(12) 0.0131(12) C10 0.0300(16) 0.0345(16) 0.0289(16) -0.0049(13) -0.0074(12) 0.0192(14) C11 0.0375(17) 0.0343(16) 0.0245(15) 0.0030(13) -0.0053(13) 0.0209(14) C12 0.0326(16) 0.0286(15) 0.0234(14) 0.0036(12) 0.0008(12) 0.0164(13) C13 0.0278(15) 0.0266(15) 0.0230(14) -0.0016(12) 0.0004(12) 0.0146(13) C14 0.0222(14) 0.0216(14) 0.0277(15) 0.0014(12) -0.0018(12) 0.0061(12) C15 0.0271(15) 0.0196(14) 0.0290(16) 0.0023(11) 0.0022(12) 0.0115(12) C16 0.0221(14) 0.0284(15) 0.0220(14) 0.0040(12) 0.0005(11) 0.0096(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C15 1.833(3) . ? Cr1 C13 1.847(3) . ? Cr1 C14 1.885(3) . ? Cr1 C16 1.919(3) . ? Cr1 N2 2.110(2) . ? Cr1 N1 2.118(2) . ? O1 C4 1.380(3) . ? O1 H1 0.8200 . ? O13 C13 1.162(3) . ? O14 C14 1.160(3) . ? O15 C15 1.170(3) . ? O16 C16 1.147(3) . ? N1 C7 1.292(3) . ? N1 C1 1.440(3) . ? N2 C12 1.345(3) . ? N2 C8 1.363(3) . ? C1 C6 1.391(4) . ? C1 C2 1.393(4) . ? C2 C3 1.387(4) . ? C2 H2 0.9300 . ? C3 C4 1.385(4) . ? C3 H3 0.9300 . ? C4 C5 1.389(4) . ? C5 C6 1.384(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.449(4) . ? C7 H7 0.9300 . ? C8 C9 1.386(4) . ? C9 C10 1.378(4) . ? C9 H9 0.9300 . ? C10 C11 1.380(4) . ? C10 H10 0.9300 . ? C11 C12 1.388(4) . ? 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 C15 Cr1 C13 89.93(12) . . ? C15 Cr1 C14 85.73(12) . . ? C13 Cr1 C14 83.57(12) . . ? C15 Cr1 C16 87.15(12) . . ? C13 Cr1 C16 86.81(11) . . ? C14 Cr1 C16 168.03(11) . . ? C15 Cr1 N2 172.38(11) . . ? C13 Cr1 N2 97.06(10) . . ? C14 Cr1 N2 98.03(10) . . ? C16 Cr1 N2 90.19(10) . . ? C15 Cr1 N1 96.97(10) . . ? C13 Cr1 N1 172.82(10) . . ? C14 Cr1 N1 94.91(10) . . ? C16 Cr1 N1 95.49(10) . . ? N2 Cr1 N1 76.16(8) . . ? C4 O1 H1 109.5 . . ? C7 N1 C1 115.8(2) . . ? C7 N1 Cr1 115.95(17) . . ? C1 N1 Cr1 128.23(16) . . ? C12 N2 C8 116.9(2) . . ? C12 N2 Cr1 127.29(18) . . ? C8 N2 Cr1 115.76(17) . . ? C6 C1 C2 119.6(2) . . ? C6 C1 N1 121.1(2) . . ? C2 C1 N1 119.2(2) . . ? C3 C2 C1 120.3(3) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 119.5(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? O1 C4 C3 118.6(3) . . ? O1 C4 C5 120.7(3) . . ? C3 C4 C5 120.6(2) . . ? C6 C5 C4 119.8(3) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 120.1(2) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? N1 C7 C8 118.0(2) . . ? N1 C7 H7 121.0 . . ? C8 C7 H7 121.0 . . ? N2 C8 C9 123.2(2) . . ? N2 C8 C7 113.7(2) . . ? C9 C8 C7 123.1(2) . . ? C10 C9 C8 119.0(3) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 118.5(3) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.7 . . ? C10 C11 C12 119.9(3) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? N2 C12 C11 122.5(3) . . ? N2 C12 H12 118.7 . . ? C11 C12 H12 118.8 . . ? O13 C13 Cr1 176.1(2) . . ? O14 C14 Cr1 170.1(2) . . ? O15 C15 Cr1 176.9(3) . . ? O16 C16 Cr1 173.0(2) . . ? 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 Cr1 N1 C7 -172.4(2) . . . . ? C13 Cr1 N1 C7 23.8(9) . . . . ? C14 Cr1 N1 C7 101.3(2) . . . . ? C16 Cr1 N1 C7 -84.6(2) . . . . ? N2 Cr1 N1 C7 4.20(18) . . . . ? C15 Cr1 N1 C1 7.4(2) . . . . ? C13 Cr1 N1 C1 -156.4(8) . . . . ? C14 Cr1 N1 C1 -78.9(2) . . . . ? C16 Cr1 N1 C1 95.2(2) . . . . ? N2 Cr1 N1 C1 -176.0(2) . . . . ? C15 Cr1 N2 C12 -156.1(7) . . . . ? C13 Cr1 N2 C12 0.3(2) . . . . ? C14 Cr1 N2 C12 84.8(2) . . . . ? C16 Cr1 N2 C12 -86.5(2) . . . . ? N1 Cr1 N2 C12 177.9(2) . . . . ? C15 Cr1 N2 C8 20.5(8) . . . . ? C13 Cr1 N2 C8 176.83(19) . . . . ? C14 Cr1 N2 C8 -98.70(19) . . . . ? C16 Cr1 N2 C8 90.02(19) . . . . ? N1 Cr1 N2 C8 -5.59(17) . . . . ? C7 N1 C1 C6 46.9(3) . . . . ? Cr1 N1 C1 C6 -132.9(2) . . . . ? C7 N1 C1 C2 -130.6(3) . . . . ? Cr1 N1 C1 C2 49.6(3) . . . . ? C6 C1 C2 C3 -2.8(4) . . . . ? N1 C1 C2 C3 174.7(2) . . . . ? C1 C2 C3 C4 1.8(4) . . . . ? C2 C3 C4 O1 179.5(3) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? O1 C4 C5 C6 179.5(3) . . . . ? C3 C4 C5 C6 -1.2(4) . . . . ? C4 C5 C6 C1 0.2(4) . . . . ? C2 C1 C6 C5 1.8(4) . . . . ? N1 C1 C6 C5 -175.7(2) . . . . ? C1 N1 C7 C8 177.8(2) . . . . ? Cr1 N1 C7 C8 -2.3(3) . . . . ? C12 N2 C8 C9 1.7(4) . . . . ? Cr1 N2 C8 C9 -175.3(2) . . . . ? C12 N2 C8 C7 -176.9(2) . . . . ? Cr1 N2 C8 C7 6.1(3) . . . . ? N1 C7 C8 N2 -2.5(3) . . . . ? N1 C7 C8 C9 178.8(2) . . . . ? N2 C8 C9 C10 -1.7(4) . . . . ? C7 C8 C9 C10 176.8(2) . . . . ? C8 C9 C10 C11 -0.1(4) . . . . ? C9 C10 C11 C12 1.8(4) . . . . ? C8 N2 C12 C11 0.2(4) . . . . ? Cr1 N2 C12 C11 176.7(2) . . . . ? C10 C11 C12 N2 -1.9(4) . . . . ? C15 Cr1 C13 O13 -32(4) . . . . ? C14 Cr1 C13 O13 54(4) . . . . ? C16 Cr1 C13 O13 -119(4) . . . . ? N2 Cr1 C13 O13 152(4) . . . . ? N1 Cr1 C13 O13 132(3) . . . . ? C15 Cr1 C14 O14 44.7(15) . . . . ? C13 Cr1 C14 O14 -45.7(14) . . . . ? C16 Cr1 C14 O14 -8.9(19) . . . . ? N2 Cr1 C14 O14 -141.9(14) . . . . ? N1 Cr1 C14 O14 141.4(14) . . . . ? C13 Cr1 C15 O15 8(5) . . . . ? C14 Cr1 C15 O15 -75(5) . . . . ? C16 Cr1 C15 O15 95(5) . . . . ? N2 Cr1 C15 O15 165(4) . . . . ? N1 Cr1 C15 O15 -170(5) . . . . ? C15 Cr1 C16 O16 -52(2) . . . . ? C13 Cr1 C16 O16 38(2) . . . . ? C14 Cr1 C16 O16 2(2) . . . . ? N2 Cr1 C16 O16 135(2) . . . . ? N1 Cr1 C16 O16 -149(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.782 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.071 #===END #============================================================================== data_ka383 _database_code_CSD 179590 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H10 N2 O5 W' _chemical_formula_weight 494.11 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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 9.0040(18) _cell_length_b 24.712(5) _cell_length_c 7.0730(14) _cell_angle_alpha 90.00 _cell_angle_beta 108.99(3) _cell_angle_gamma 90.00 _cell_volume 1488.1(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 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 7.793 _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 8040 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_sigmaI/netI 0.0866 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 30.07 _reflns_number_total 4338 _reflns_number_gt 3002 _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^)+(0.0542P)^2^+5.8294P] 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 4338 _refine_ls_number_parameters 222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1325 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.85195(3) 0.114754(13) 0.10535(5) 0.02883(12) Uani 1 1 d . . . O1 O 0.3126(8) 0.3358(3) -0.1297(10) 0.0442(16) Uani 1 1 d . . . O13 O 1.1702(7) 0.0573(3) 0.1460(10) 0.0445(16) Uani 1 1 d . . . O14 O 0.7748(8) 0.0751(3) -0.3407(10) 0.0489(17) Uani 1 1 d . . . O15 O 0.9525(7) 0.2214(3) -0.0603(10) 0.0424(15) Uani 1 1 d . . . O16 O 0.9954(8) 0.1618(3) 0.5477(10) 0.0462(16) Uani 1 1 d . . . N1 N 0.6064(7) 0.1357(3) 0.0921(10) 0.0285(14) Uani 1 1 d . . . N2 N 0.7526(7) 0.0421(3) 0.2067(10) 0.0297(14) Uani 1 1 d . . . C1 C 0.5267(9) 0.1868(3) 0.0266(12) 0.0305(17) Uani 1 1 d . . . C2 C 0.6113(9) 0.2349(4) 0.0852(13) 0.0340(18) Uani 1 1 d . . . H2 H 0.7173 0.2336 0.1606 0.045(9) Uiso 1 1 calc R . . C3 C 0.5382(10) 0.2841(4) 0.0319(13) 0.0359(19) Uani 1 1 d . . . H3 H 0.5942 0.3161 0.0706 0.045(9) Uiso 1 1 calc R . . C4 C 0.3810(10) 0.2854(3) -0.0796(13) 0.0338(18) Uani 1 1 d . . . C5 C 0.2961(9) 0.2388(4) -0.1431(13) 0.0343(19) Uani 1 1 d . . . H5 H 0.1910 0.2405 -0.2221 0.045(9) Uiso 1 1 calc R . . C6 C 0.3695(9) 0.1892(4) -0.0877(12) 0.0311(17) Uani 1 1 d . . . H6 H 0.3128 0.1574 -0.1276 0.045(9) Uiso 1 1 calc R . . C7 C 0.5285(9) 0.0987(4) 0.1413(12) 0.0326(18) Uani 1 1 d . . . H7 H 0.4251 0.1049 0.1354 0.045(9) Uiso 1 1 calc R . . C8 C 0.6027(9) 0.0463(4) 0.2074(12) 0.0309(17) Uani 1 1 d . . . C9 C 0.5244(10) 0.0042(3) 0.2660(13) 0.0344(18) Uani 1 1 d . . . H9 H 0.4201 0.0078 0.2598 0.045(9) Uiso 1 1 calc R . . C10 C 0.6069(10) -0.0436(4) 0.3343(14) 0.038(2) Uani 1 1 d . . . H10 H 0.5591 -0.0722 0.3779 0.045(9) Uiso 1 1 calc R . . C11 C 0.7608(10) -0.0481(4) 0.3365(13) 0.038(2) Uani 1 1 d . . . H11 H 0.8187 -0.0795 0.3812 0.045(9) Uiso 1 1 calc R . . C12 C 0.8248(10) -0.0045(4) 0.2700(14) 0.038(2) Uani 1 1 d . . . H12 H 0.9275 -0.0079 0.2694 0.045(9) Uiso 1 1 calc R . . C13 C 1.0541(9) 0.0809(3) 0.1312(13) 0.0334(18) Uani 1 1 d . . . C14 C 0.7928(9) 0.0880(4) -0.1817(12) 0.0333(18) Uani 1 1 d . . . C15 C 0.9163(9) 0.1825(4) 0.0063(13) 0.0345(19) Uani 1 1 d . . . C16 C 0.9392(9) 0.1453(4) 0.3930(13) 0.0344(19) Uani 1 1 d . . . H1 H 0.208(10) 0.338(3) -0.139(12) 0.03(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 W1 0.02214(16) 0.03245(19) 0.03177(19) -0.00181(15) 0.00858(12) -0.00021(14) O1 0.036(3) 0.043(4) 0.055(4) 0.011(3) 0.017(3) 0.006(3) O13 0.027(3) 0.057(4) 0.053(4) -0.003(3) 0.017(3) 0.003(3) O14 0.050(4) 0.066(5) 0.035(4) -0.006(3) 0.019(3) -0.011(4) O15 0.039(3) 0.040(4) 0.050(4) 0.001(3) 0.018(3) -0.003(3) O16 0.049(4) 0.046(4) 0.037(4) -0.008(3) 0.004(3) 0.001(3) N1 0.025(3) 0.032(4) 0.032(4) -0.002(3) 0.014(3) -0.001(3) N2 0.027(3) 0.029(4) 0.032(4) 0.000(3) 0.006(3) 0.003(3) C1 0.032(4) 0.033(4) 0.031(4) 0.002(3) 0.016(3) 0.003(3) C2 0.027(4) 0.041(5) 0.033(4) -0.004(4) 0.008(3) -0.003(4) C3 0.035(4) 0.036(5) 0.039(5) 0.000(4) 0.015(4) -0.004(4) C4 0.036(4) 0.035(5) 0.033(5) 0.007(4) 0.016(4) 0.005(4) C5 0.021(4) 0.042(5) 0.039(5) 0.005(4) 0.009(3) 0.006(3) C6 0.025(4) 0.039(5) 0.029(4) 0.006(3) 0.008(3) 0.000(3) C7 0.025(4) 0.043(5) 0.031(4) -0.010(3) 0.010(3) 0.001(3) C8 0.023(4) 0.041(5) 0.027(4) -0.007(3) 0.006(3) -0.004(3) C9 0.033(4) 0.039(5) 0.033(5) 0.001(4) 0.014(4) -0.001(4) C10 0.035(4) 0.040(5) 0.044(5) 0.002(4) 0.017(4) -0.001(4) C11 0.042(5) 0.028(4) 0.039(5) 0.006(4) 0.007(4) 0.009(4) C12 0.028(4) 0.035(5) 0.047(5) -0.005(4) 0.006(4) 0.005(4) C13 0.029(4) 0.034(5) 0.038(5) -0.012(4) 0.013(4) -0.007(4) C14 0.028(4) 0.046(5) 0.028(4) -0.001(4) 0.012(3) -0.004(4) C15 0.023(4) 0.040(5) 0.037(5) -0.004(4) 0.005(3) 0.000(3) C16 0.025(4) 0.042(5) 0.039(5) 0.002(4) 0.014(4) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C13 1.956(8) . ? W1 C15 1.974(9) . ? W1 C14 2.035(8) . ? W1 C16 2.070(9) . ? W1 N2 2.226(7) . ? W1 N1 2.243(6) . ? O1 C4 1.382(10) . ? O1 H1 0.92(9) . ? O13 C13 1.172(9) . ? O14 C14 1.129(10) . ? O15 C15 1.163(10) . ? O16 C16 1.122(10) . ? N1 C7 1.267(11) . ? N1 C1 1.452(10) . ? N2 C12 1.326(11) . ? N2 C8 1.356(10) . ? C1 C6 1.384(11) . ? C1 C2 1.400(11) . ? C2 C3 1.376(12) . ? C2 H2 0.9300 . ? C3 C4 1.379(12) . ? C3 H3 0.9300 . ? C4 C5 1.375(12) . ? C5 C6 1.386(11) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.462(12) . ? C7 H7 0.9300 . ? C8 C9 1.395(11) . ? C9 C10 1.395(12) . ? C9 H9 0.9300 . ? C10 C11 1.385(12) . ? C10 H10 0.9300 . ? C11 C12 1.376(13) . ? 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 W1 C15 91.4(3) . . ? C13 W1 C14 83.6(3) . . ? C15 W1 C14 86.2(4) . . ? C13 W1 C16 91.1(3) . . ? C15 W1 C16 88.8(3) . . ? C14 W1 C16 172.6(3) . . ? C13 W1 N2 94.9(3) . . ? C15 W1 N2 173.7(3) . . ? C14 W1 N2 93.3(3) . . ? C16 W1 N2 92.4(3) . . ? C13 W1 N1 167.7(3) . . ? C15 W1 N1 100.9(3) . . ? C14 W1 N1 95.7(3) . . ? C16 W1 N1 90.6(3) . . ? N2 W1 N1 72.9(2) . . ? C4 O1 H1 115(5) . . ? C7 N1 C1 117.0(7) . . ? C7 N1 W1 116.6(6) . . ? C1 N1 W1 126.3(5) . . ? C12 N2 C8 116.4(7) . . ? C12 N2 W1 127.2(6) . . ? C8 N2 W1 116.4(5) . . ? C6 C1 C2 119.3(8) . . ? C6 C1 N1 122.0(7) . . ? C2 C1 N1 118.7(7) . . ? C3 C2 C1 120.3(8) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 119.2(8) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 121.7(8) . . ? C5 C4 O1 121.1(8) . . ? C3 C4 O1 117.2(8) . . ? C4 C5 C6 119.0(8) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C1 C6 C5 120.4(8) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? N1 C7 C8 119.3(7) . . ? N1 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? N2 C8 C9 123.0(8) . . ? N2 C8 C7 114.8(7) . . ? C9 C8 C7 122.3(7) . . ? C8 C9 C10 118.1(8) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? C11 C10 C9 119.4(8) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C12 C11 C10 117.5(8) . . ? C12 C11 H11 121.3 . . ? C10 C11 H11 121.3 . . ? N2 C12 C11 125.6(8) . . ? N2 C12 H12 117.2 . . ? C11 C12 H12 117.2 . . ? O13 C13 W1 175.4(7) . . ? O14 C14 W1 172.8(7) . . ? O15 C15 W1 177.0(8) . . ? O16 C16 W1 175.8(7) . . ? 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 W1 N1 C7 4.5(17) . . . . ? C15 W1 N1 C7 177.6(6) . . . . ? C14 W1 N1 C7 90.4(6) . . . . ? C16 W1 N1 C7 -93.6(6) . . . . ? N2 W1 N1 C7 -1.3(6) . . . . ? C13 W1 N1 C1 -173.3(12) . . . . ? C15 W1 N1 C1 -0.2(7) . . . . ? C14 W1 N1 C1 -87.4(6) . . . . ? C16 W1 N1 C1 88.6(7) . . . . ? N2 W1 N1 C1 -179.1(7) . . . . ? C13 W1 N2 C12 3.4(7) . . . . ? C15 W1 N2 C12 172(3) . . . . ? C14 W1 N2 C12 87.2(7) . . . . ? C16 W1 N2 C12 -88.0(7) . . . . ? N1 W1 N2 C12 -177.9(8) . . . . ? C13 W1 N2 C8 -178.0(6) . . . . ? C15 W1 N2 C8 -9(3) . . . . ? C14 W1 N2 C8 -94.2(6) . . . . ? C16 W1 N2 C8 90.7(6) . . . . ? N1 W1 N2 C8 0.7(5) . . . . ? C7 N1 C1 C6 -37.3(11) . . . . ? W1 N1 C1 C6 140.5(6) . . . . ? C7 N1 C1 C2 141.2(8) . . . . ? W1 N1 C1 C2 -41.0(10) . . . . ? C6 C1 C2 C3 0.8(12) . . . . ? N1 C1 C2 C3 -177.7(7) . . . . ? C1 C2 C3 C4 0.1(12) . . . . ? C2 C3 C4 C5 -1.6(13) . . . . ? C2 C3 C4 O1 180.0(8) . . . . ? C3 C4 C5 C6 2.2(13) . . . . ? O1 C4 C5 C6 -179.5(7) . . . . ? C2 C1 C6 C5 -0.3(12) . . . . ? N1 C1 C6 C5 178.2(7) . . . . ? C4 C5 C6 C1 -1.2(12) . . . . ? C1 N1 C7 C8 179.7(7) . . . . ? W1 N1 C7 C8 1.6(10) . . . . ? C12 N2 C8 C9 -1.5(12) . . . . ? W1 N2 C8 C9 179.7(6) . . . . ? C12 N2 C8 C7 178.5(7) . . . . ? W1 N2 C8 C7 -0.2(9) . . . . ? N1 C7 C8 N2 -0.9(11) . . . . ? N1 C7 C8 C9 179.1(8) . . . . ? N2 C8 C9 C10 2.6(13) . . . . ? C7 C8 C9 C10 -177.5(8) . . . . ? C8 C9 C10 C11 -1.7(13) . . . . ? C9 C10 C11 C12 0.0(14) . . . . ? C8 N2 C12 C11 -0.4(13) . . . . ? W1 N2 C12 C11 178.2(7) . . . . ? C10 C11 C12 N2 1.1(15) . . . . ? C15 W1 C13 O13 -158(9) . . . . ? C14 W1 C13 O13 -72(9) . . . . ? C16 W1 C13 O13 113(9) . . . . ? N2 W1 C13 O13 21(9) . . . . ? N1 W1 C13 O13 15(10) . . . . ? C13 W1 C14 O14 -44(7) . . . . ? C15 W1 C14 O14 47(7) . . . . ? C16 W1 C14 O14 0(9) . . . . ? N2 W1 C14 O14 -139(7) . . . . ? N1 W1 C14 O14 148(7) . . . . ? C13 W1 C15 O15 81(13) . . . . ? C14 W1 C15 O15 -2(13) . . . . ? C16 W1 C15 O15 173(13) . . . . ? N2 W1 C15 O15 -87(14) . . . . ? N1 W1 C15 O15 -97(13) . . . . ? C13 W1 C16 O16 28(11) . . . . ? C15 W1 C16 O16 -63(11) . . . . ? C14 W1 C16 O16 -17(12) . . . . ? N2 W1 C16 O16 123(11) . . . . ? N1 W1 C16 O16 -164(11) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.500 _refine_diff_density_min -1.467 _refine_diff_density_rms 0.233 #===END #============================================================================== data_ka380 _database_code_CSD 179591 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H19 Cr N3 O4' _chemical_formula_weight 417.38 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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.469(2) _cell_length_b 12.979(3) _cell_length_c 13.105(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.81(3) _cell_angle_gamma 90.00 _cell_volume 1949.8(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 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.618 _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 10810 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 30.03 _reflns_number_total 5681 _reflns_number_gt 4157 _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^)+(0.0503P)^2^+0.4056P] 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 5681 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1088 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.39752(2) 0.88934(2) 0.17574(2) 0.01701(9) Uani 1 1 d . . . O1 O -0.20774(12) 0.83847(11) 0.11996(12) 0.0290(3) Uani 1 1 d . . . O13 O 0.60880(12) 1.02639(10) 0.17149(11) 0.0323(3) Uani 1 1 d . . . O14 O 0.47083(15) 0.80863(11) -0.02882(11) 0.0406(4) Uani 1 1 d . . . O15 O 0.26593(12) 1.05573(10) 0.06307(10) 0.0294(3) Uani 1 1 d . . . N1 N 0.26891(12) 0.77541(11) 0.19096(11) 0.0178(3) Uani 1 1 d . . . N2 N 0.48749(12) 0.76403(11) 0.24599(11) 0.0184(3) Uani 1 1 d . . . N3 N 0.30798(14) 0.95932(12) 0.39213(12) 0.0257(3) Uani 1 1 d . . . C1 C 0.14665(15) 0.78974(13) 0.17097(13) 0.0187(3) Uani 1 1 d . . . C2 C 0.10713(16) 0.83154(14) 0.07889(14) 0.0207(4) Uani 1 1 d . . . C3 C -0.01102(16) 0.84672(14) 0.05869(15) 0.0227(4) Uani 1 1 d . . . C4 C -0.09052(15) 0.82243(13) 0.13314(14) 0.0221(4) Uani 1 1 d . . . C5 C -0.05138(16) 0.78259(15) 0.22615(15) 0.0248(4) Uani 1 1 d . . . C6 C 0.06611(16) 0.76441(15) 0.24440(14) 0.0227(4) Uani 1 1 d . . . C7 C 0.30168(16) 0.68852(13) 0.22995(14) 0.0204(4) Uani 1 1 d . . . C8 C 0.42436(15) 0.67592(13) 0.25600(13) 0.0191(3) Uani 1 1 d . . . C9 C 0.47484(17) 0.58258(14) 0.28555(15) 0.0238(4) Uani 1 1 d . . . C10 C 0.59354(17) 0.57983(15) 0.30846(15) 0.0258(4) Uani 1 1 d . . . C11 C 0.65692(16) 0.66953(15) 0.30242(15) 0.0244(4) Uani 1 1 d . . . C12 C 0.60166(16) 0.75994(14) 0.27060(14) 0.0228(4) Uani 1 1 d . . . C13 C 0.52628(16) 0.97460(13) 0.17519(14) 0.0226(4) Uani 1 1 d . . . C14 C 0.44223(16) 0.83901(14) 0.04920(15) 0.0238(4) Uani 1 1 d . . . C15 C 0.31497(15) 0.98932(13) 0.10794(14) 0.0203(4) Uani 1 1 d . . . C16 C 0.34502(15) 0.93717(13) 0.31383(14) 0.0214(4) Uani 1 1 d . . . C17 C 0.26013(18) 0.96967(15) 0.49438(14) 0.0283(4) Uani 1 1 d . . . C18 C 0.1624(2) 0.8890(2) 0.5023(2) 0.0435(6) Uani 1 1 d . . . C19 C 0.2100(3) 1.0788(2) 0.5064(2) 0.0474(6) Uani 1 1 d . . . C20 C 0.3583(2) 0.9497(2) 0.57174(19) 0.0459(6) Uani 1 1 d . . . H1 H -0.224(2) 0.8652(19) 0.071(2) 0.041(8) Uiso 1 1 d . . . H2 H 0.1587(18) 0.8484(16) 0.0323(16) 0.030(6) Uiso 1 1 d . . . H3 H -0.0397(18) 0.8758(16) -0.0018(17) 0.030(6) Uiso 1 1 d . . . H5 H -0.1027(18) 0.7712(16) 0.2787(16) 0.029(6) Uiso 1 1 d . . . H6 H 0.0902(18) 0.7402(18) 0.3024(17) 0.033(6) Uiso 1 1 d . . . H7 H 0.2500(18) 0.6320(16) 0.2404(15) 0.027(5) Uiso 1 1 d . . . H9 H 0.4291(18) 0.5260(16) 0.2889(16) 0.025(5) Uiso 1 1 d . . . H10 H 0.6293(18) 0.5178(18) 0.3280(16) 0.033(6) Uiso 1 1 d . . . H11 H 0.734(2) 0.6705(16) 0.3165(17) 0.036(6) Uiso 1 1 d . . . H12 H 0.6458(17) 0.8238(15) 0.2601(15) 0.025(5) Uiso 1 1 d . . . H1A H 0.202(2) 0.814(2) 0.496(2) 0.063(8) Uiso 1 1 d . . . H1B H 0.097(2) 0.9094(19) 0.451(2) 0.049(7) Uiso 1 1 d . . . H1C H 0.130(2) 0.8985(19) 0.560(2) 0.049(8) Uiso 1 1 d . . . H2A H 0.141(3) 1.083(2) 0.456(2) 0.075(10) Uiso 1 1 d . . . H2B H 0.274(2) 1.126(2) 0.4997(19) 0.049(8) Uiso 1 1 d . . . H2C H 0.1840(17) 1.0927(15) 0.5653(17) 0.017(5) Uiso 1 1 d . . . H3A H 0.392(2) 0.877(2) 0.555(2) 0.051(7) Uiso 1 1 d . . . H3B H 0.422(2) 1.005(2) 0.562(2) 0.060(8) Uiso 1 1 d . . . H3C H 0.324(2) 0.948(2) 0.640(2) 0.064(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 Cr1 0.01742(15) 0.01600(14) 0.01759(15) 0.00150(11) 0.00015(10) 0.00028(11) O1 0.0187(7) 0.0360(8) 0.0320(8) 0.0078(7) -0.0030(6) 0.0001(6) O13 0.0271(7) 0.0296(7) 0.0399(9) 0.0051(6) -0.0029(6) -0.0086(6) O14 0.0605(11) 0.0376(8) 0.0244(8) 0.0004(6) 0.0125(7) 0.0118(8) O15 0.0300(7) 0.0280(7) 0.0300(8) 0.0074(6) -0.0011(6) 0.0084(6) N1 0.0187(7) 0.0188(7) 0.0160(7) -0.0001(6) -0.0002(6) -0.0003(6) N2 0.0195(7) 0.0185(7) 0.0172(7) 0.0013(6) 0.0006(6) 0.0014(6) N3 0.0326(9) 0.0230(8) 0.0216(8) -0.0007(6) 0.0004(7) 0.0031(7) C1 0.0180(8) 0.0183(8) 0.0197(9) -0.0015(7) -0.0018(7) -0.0010(7) C2 0.0206(9) 0.0231(9) 0.0185(9) 0.0013(7) 0.0019(7) -0.0007(7) C3 0.0230(9) 0.0232(9) 0.0215(9) 0.0038(7) -0.0034(7) -0.0011(7) C4 0.0193(8) 0.0199(8) 0.0270(10) -0.0008(7) -0.0020(7) -0.0013(7) C5 0.0216(9) 0.0295(10) 0.0235(10) 0.0042(8) 0.0019(8) -0.0025(8) C6 0.0218(9) 0.0268(9) 0.0193(9) 0.0039(7) -0.0024(7) -0.0029(7) C7 0.0227(9) 0.0182(8) 0.0200(9) 0.0006(7) -0.0009(7) -0.0029(7) C8 0.0214(8) 0.0187(8) 0.0171(9) 0.0001(6) 0.0004(7) 0.0010(7) C9 0.0254(10) 0.0180(8) 0.0280(10) 0.0033(7) -0.0002(8) -0.0007(7) C10 0.0273(10) 0.0218(9) 0.0284(11) 0.0060(8) 0.0024(8) 0.0073(8) C11 0.0175(9) 0.0297(9) 0.0259(10) 0.0041(8) 0.0016(7) 0.0045(8) C12 0.0203(9) 0.0229(9) 0.0251(10) 0.0036(7) 0.0005(7) 0.0005(7) C13 0.0253(9) 0.0205(8) 0.0220(9) 0.0029(7) -0.0011(7) 0.0029(7) C14 0.0257(9) 0.0208(9) 0.0250(10) 0.0039(7) 0.0011(8) 0.0027(7) C15 0.0186(8) 0.0217(8) 0.0206(9) -0.0014(7) 0.0017(7) -0.0001(7) C16 0.0227(9) 0.0165(8) 0.0247(10) 0.0011(7) -0.0050(7) 0.0008(7) C17 0.0384(11) 0.0285(10) 0.0183(10) -0.0007(8) 0.0039(8) 0.0008(9) C18 0.0512(15) 0.0496(15) 0.0298(13) -0.0002(11) 0.0059(11) -0.0154(13) C19 0.0670(19) 0.0375(13) 0.0387(15) -0.0004(11) 0.0178(14) 0.0063(13) C20 0.0509(15) 0.0602(17) 0.0262(13) 0.0020(11) -0.0059(11) -0.0044(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C15 1.8212(18) . ? Cr1 C13 1.8456(19) . ? Cr1 C14 1.869(2) . ? Cr1 C16 2.023(2) . ? Cr1 N1 2.1025(14) . ? Cr1 N2 2.1207(15) . ? O1 C4 1.366(2) . ? O1 H1 0.75(3) . ? O13 C13 1.163(2) . ? O14 C14 1.153(2) . ? O15 C15 1.176(2) . ? N1 C7 1.289(2) . ? N1 C1 1.430(2) . ? N2 C12 1.340(2) . ? N2 C8 1.362(2) . ? N3 C16 1.159(2) . ? N3 C17 1.470(2) . ? C1 C2 1.386(2) . ? C1 C6 1.394(3) . ? C2 C3 1.386(3) . ? C2 H2 0.89(2) . ? C3 C4 1.392(3) . ? C3 H3 0.93(2) . ? C4 C5 1.386(3) . ? C5 C6 1.381(3) . ? C5 H5 0.93(2) . ? C6 H6 0.86(2) . ? C7 C8 1.447(2) . ? C7 H7 0.96(2) . ? C8 C9 1.392(2) . ? C9 C10 1.385(3) . ? C9 H9 0.90(2) . ? C10 C11 1.376(3) . ? C10 H10 0.93(2) . ? C11 C12 1.391(3) . ? C11 H11 0.90(2) . ? C12 H12 0.98(2) . ? C17 C20 1.513(3) . ? C17 C19 1.539(3) . ? C17 C18 1.540(3) . ? C18 H1A 1.07(3) . ? C18 H1B 1.03(3) . ? C18 H1C 0.86(3) . ? C19 H2A 1.02(3) . ? C19 H2B 0.97(3) . ? C19 H2C 0.86(2) . ? C20 H3A 1.04(3) . ? C20 H3B 1.04(3) . ? C20 H3C 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 Cr1 C13 88.54(8) . . ? C15 Cr1 C14 88.23(8) . . ? C13 Cr1 C14 87.94(8) . . ? C15 Cr1 C16 93.03(8) . . ? C13 Cr1 C16 94.61(8) . . ? C14 Cr1 C16 177.18(8) . . ? C15 Cr1 N1 101.06(7) . . ? C13 Cr1 N1 170.37(7) . . ? C14 Cr1 N1 92.95(7) . . ? C16 Cr1 N1 84.34(7) . . ? C15 Cr1 N2 175.26(7) . . ? C13 Cr1 N2 94.77(7) . . ? C14 Cr1 N2 88.49(7) . . ? C16 Cr1 N2 90.09(6) . . ? N1 Cr1 N2 75.68(6) . . ? C4 O1 H1 114(2) . . ? C7 N1 C1 117.26(15) . . ? C7 N1 Cr1 117.14(12) . . ? C1 N1 Cr1 125.30(11) . . ? C12 N2 C8 117.52(15) . . ? C12 N2 Cr1 126.40(12) . . ? C8 N2 Cr1 115.65(11) . . ? C16 N3 C17 170.88(18) . . ? C2 C1 C6 119.19(16) . . ? C2 C1 N1 120.13(16) . . ? C6 C1 N1 120.66(16) . . ? C1 C2 C3 120.83(17) . . ? C1 C2 H2 119.2(14) . . ? C3 C2 H2 120.0(14) . . ? C2 C3 C4 119.46(17) . . ? C2 C3 H3 122.6(13) . . ? C4 C3 H3 117.9(13) . . ? O1 C4 C5 117.28(17) . . ? O1 C4 C3 122.72(17) . . ? C5 C4 C3 119.98(17) . . ? C6 C5 C4 120.21(18) . . ? C6 C5 H5 118.7(13) . . ? C4 C5 H5 121.0(13) . . ? C5 C6 C1 120.28(17) . . ? C5 C6 H6 120.0(14) . . ? C1 C6 H6 119.7(14) . . ? N1 C7 C8 117.49(16) . . ? N1 C7 H7 123.7(12) . . ? C8 C7 H7 118.8(12) . . ? N2 C8 C9 122.66(16) . . ? N2 C8 C7 113.47(15) . . ? C9 C8 C7 123.83(16) . . ? C10 C9 C8 118.67(17) . . ? C10 C9 H9 122.5(13) . . ? C8 C9 H9 118.9(13) . . ? C11 C10 C9 118.89(18) . . ? C11 C10 H10 121.1(13) . . ? C9 C10 H10 120.0(13) . . ? C10 C11 C12 119.62(18) . . ? C10 C11 H11 121.3(14) . . ? C12 C11 H11 119.1(14) . . ? N2 C12 C11 122.55(17) . . ? N2 C12 H12 115.9(11) . . ? C11 C12 H12 121.4(11) . . ? O13 C13 Cr1 177.37(17) . . ? O14 C14 Cr1 179.28(18) . . ? O15 C15 Cr1 177.24(16) . . ? N3 C16 Cr1 174.79(16) . . ? N3 C17 C20 107.68(18) . . ? N3 C17 C19 109.19(17) . . ? C20 C17 C19 111.2(2) . . ? N3 C17 C18 107.03(17) . . ? C20 C17 C18 111.5(2) . . ? C19 C17 C18 110.1(2) . . ? C17 C18 H1A 107.5(14) . . ? C17 C18 H1B 107.5(14) . . ? H1A C18 H1B 119(2) . . ? C17 C18 H1C 107.1(17) . . ? H1A C18 H1C 113(2) . . ? H1B C18 H1C 102(2) . . ? C17 C19 H2A 105.7(18) . . ? C17 C19 H2B 106.9(16) . . ? H2A C19 H2B 119(2) . . ? C17 C19 H2C 115.4(13) . . ? H2A C19 H2C 107(2) . . ? H2B C19 H2C 104(2) . . ? C17 C20 H3A 106.6(15) . . ? C17 C20 H3B 108.3(15) . . ? H3A C20 H3B 109(2) . . ? C17 C20 H3C 107.4(16) . . ? H3A C20 H3C 109(2) . . ? H3B C20 H3C 116(2) . . ? 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 Cr1 N1 C7 174.76(13) . . . . ? C13 Cr1 N1 C7 -9.1(5) . . . . ? C14 Cr1 N1 C7 85.98(14) . . . . ? C16 Cr1 N1 C7 -93.25(14) . . . . ? N2 Cr1 N1 C7 -1.71(13) . . . . ? C15 Cr1 N1 C1 -11.70(14) . . . . ? C13 Cr1 N1 C1 164.5(4) . . . . ? C14 Cr1 N1 C1 -100.47(14) . . . . ? C16 Cr1 N1 C1 80.29(14) . . . . ? N2 Cr1 N1 C1 171.84(14) . . . . ? C15 Cr1 N2 C12 130.8(8) . . . . ? C13 Cr1 N2 C12 -3.38(16) . . . . ? C14 Cr1 N2 C12 84.43(16) . . . . ? C16 Cr1 N2 C12 -98.01(15) . . . . ? N1 Cr1 N2 C12 177.85(16) . . . . ? C15 Cr1 N2 C8 -41.4(9) . . . . ? C13 Cr1 N2 C8 -175.58(13) . . . . ? C14 Cr1 N2 C8 -87.78(13) . . . . ? C16 Cr1 N2 C8 89.79(13) . . . . ? N1 Cr1 N2 C8 5.65(12) . . . . ? C7 N1 C1 C2 -134.69(18) . . . . ? Cr1 N1 C1 C2 51.8(2) . . . . ? C7 N1 C1 C6 46.9(2) . . . . ? Cr1 N1 C1 C6 -126.61(15) . . . . ? C6 C1 C2 C3 -1.0(3) . . . . ? N1 C1 C2 C3 -179.45(16) . . . . ? C1 C2 C3 C4 1.9(3) . . . . ? C2 C3 C4 O1 177.80(17) . . . . ? C2 C3 C4 C5 -0.6(3) . . . . ? O1 C4 C5 C6 179.92(17) . . . . ? C3 C4 C5 C6 -1.6(3) . . . . ? C4 C5 C6 C1 2.5(3) . . . . ? C2 C1 C6 C5 -1.2(3) . . . . ? N1 C1 C6 C5 177.22(16) . . . . ? C1 N1 C7 C8 -176.38(15) . . . . ? Cr1 N1 C7 C8 -2.3(2) . . . . ? C12 N2 C8 C9 -3.2(3) . . . . ? Cr1 N2 C8 C9 169.73(14) . . . . ? C12 N2 C8 C7 178.64(15) . . . . ? Cr1 N2 C8 C7 -8.43(19) . . . . ? N1 C7 C8 N2 7.1(2) . . . . ? N1 C7 C8 C9 -171.00(17) . . . . ? N2 C8 C9 C10 1.9(3) . . . . ? C7 C8 C9 C10 179.83(17) . . . . ? C8 C9 C10 C11 0.8(3) . . . . ? C9 C10 C11 C12 -2.0(3) . . . . ? C8 N2 C12 C11 2.0(3) . . . . ? Cr1 N2 C12 C11 -170.12(14) . . . . ? C10 C11 C12 N2 0.6(3) . . . . ? C15 Cr1 C13 O13 -95(4) . . . . ? C14 Cr1 C13 O13 -7(4) . . . . ? C16 Cr1 C13 O13 172(4) . . . . ? N1 Cr1 C13 O13 88(4) . . . . ? N2 Cr1 C13 O13 81(4) . . . . ? C15 Cr1 C14 O14 90(15) . . . . ? C13 Cr1 C14 O14 1(15) . . . . ? C16 Cr1 C14 O14 -154(15) . . . . ? N1 Cr1 C14 O14 -169(100) . . . . ? N2 Cr1 C14 O14 -94(15) . . . . ? C13 Cr1 C15 O15 18(3) . . . . ? C14 Cr1 C15 O15 -70(3) . . . . ? C16 Cr1 C15 O15 112(3) . . . . ? N1 Cr1 C15 O15 -163(3) . . . . ? N2 Cr1 C15 O15 -117(3) . . . . ? C17 N3 C16 Cr1 48(3) . . . . ? C15 Cr1 C16 N3 92.0(17) . . . . ? C13 Cr1 C16 N3 -179(100) . . . . ? C14 Cr1 C16 N3 -25(3) . . . . ? N1 Cr1 C16 N3 -8.8(17) . . . . ? N2 Cr1 C16 N3 -84.4(17) . . . . ? C16 N3 C17 C20 76.6(12) . . . . ? C16 N3 C17 C19 -162.5(11) . . . . ? C16 N3 C17 C18 -43.4(12) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.321 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.067 #===END #============================================================================== data_ka381 _database_code_CSD 179592 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H19 N3 O4 W' _chemical_formula_weight 549.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.578(2) _cell_length_b 12.995(3) _cell_length_c 13.271(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.19(3) _cell_angle_gamma 90.00 _cell_volume 1995.2(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 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 5.820 _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 10638 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.1266 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 30.04 _reflns_number_total 5837 _reflns_number_gt 3822 _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^)+(0.0598P)^2^+35.0283P] 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 5837 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1248 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.1870 _refine_ls_wR_factor_gt 0.1703 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.201 _refine_ls_shift/su_mean 0.004 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 W1 W 0.39671(4) 0.89425(3) 0.17333(3) 0.01754(14) Uani 1 1 d . . . O1 O -0.2068(7) 0.8294(8) 0.1263(8) 0.031(2) Uani 1 1 d . . . O13 O 0.6204(8) 1.0309(7) 0.1701(7) 0.033(2) Uani 1 1 d . . . O14 O 0.4762(9) 0.8041(8) -0.0325(7) 0.041(2) Uani 1 1 d . . . O15 O 0.2566(7) 1.0616(7) 0.0519(6) 0.029(2) Uani 1 1 d . . . N1 N 0.2660(8) 0.7712(7) 0.1949(6) 0.0161(18) Uani 1 1 d . . . N2 N 0.4865(8) 0.7607(7) 0.2499(7) 0.0179(19) Uani 1 1 d . . . N3 N 0.3055(9) 0.9652(9) 0.3961(8) 0.029(2) Uani 1 1 d . . . C1 C 0.1458(9) 0.7840(8) 0.1763(8) 0.019(2) Uani 1 1 d . . . C2 C 0.1035(10) 0.8272(9) 0.0850(8) 0.019(2) Uani 1 1 d . . . H2 H 0.1552 0.8472 0.0368 0.029(12) Uiso 1 1 calc R . . C3 C -0.0121(10) 0.8402(9) 0.0663(9) 0.024(2) Uani 1 1 d . . . H3 H -0.0384 0.8662 0.0043 0.029(12) Uiso 1 1 calc R . . C4 C -0.0908(9) 0.8151(9) 0.1382(9) 0.022(2) Uani 1 1 d . . . C5 C -0.0505(10) 0.7730(10) 0.2302(9) 0.028(3) Uani 1 1 d . . . H5 H -0.1025 0.7552 0.2790 0.029(12) Uiso 1 1 calc R . . C6 C 0.0653(10) 0.7581(10) 0.2478(9) 0.025(3) Uani 1 1 d . . . H6 H 0.0912 0.7300 0.3090 0.029(12) Uiso 1 1 calc R . . C7 C 0.3006(10) 0.6867(9) 0.2368(8) 0.020(2) Uani 1 1 d . . . H7 H 0.2486 0.6345 0.2504 0.029(12) Uiso 1 1 calc R . . C8 C 0.4217(10) 0.6752(10) 0.2619(8) 0.022(2) Uani 1 1 d . . . C9 C 0.4720(10) 0.5824(9) 0.2943(9) 0.024(3) Uani 1 1 d . . . H9 H 0.4265 0.5239 0.3005 0.029(12) Uiso 1 1 calc R . . C10 C 0.5903(10) 0.5779(10) 0.3173(9) 0.027(3) Uani 1 1 d . . . H10 H 0.6256 0.5170 0.3386 0.029(12) Uiso 1 1 calc R . . C11 C 0.6529(10) 0.6677(9) 0.3072(9) 0.024(2) Uani 1 1 d . . . H11 H 0.7316 0.6688 0.3241 0.029(12) Uiso 1 1 calc R . . C12 C 0.5990(11) 0.7543(10) 0.2725(9) 0.026(3) Uani 1 1 d . . . H12 H 0.6437 0.8129 0.2641 0.029(12) Uiso 1 1 calc R . . C13 C 0.5339(10) 0.9830(9) 0.1723(9) 0.022(2) Uani 1 1 d . . . C14 C 0.4452(11) 0.8379(10) 0.0423(8) 0.024(3) Uani 1 1 d . . . C15 C 0.3101(9) 0.9986(9) 0.0986(8) 0.020(2) Uani 1 1 d . . . C16 C 0.3413(10) 0.9455(9) 0.3193(8) 0.022(2) Uani 1 1 d . . . C17 C 0.2583(11) 0.9774(10) 0.4969(9) 0.028(3) Uani 1 1 d . . . C18 C 0.1645(14) 0.8952(12) 0.5043(11) 0.043(4) Uani 1 1 d . . . H18A H 0.1075 0.9046 0.4507 0.039(14) Uiso 1 1 calc R . . H18B H 0.1286 0.9011 0.5680 0.039(14) Uiso 1 1 calc R . . H18C H 0.1987 0.8282 0.4988 0.039(14) Uiso 1 1 calc R . . C19 C 0.2033(14) 1.0825(12) 0.5018(12) 0.046(4) Uani 1 1 d . . . H19A H 0.2566 1.1334 0.4792 0.039(14) Uiso 1 1 calc R . . H19B H 0.1840 1.0972 0.5700 0.039(14) Uiso 1 1 calc R . . H19C H 0.1344 1.0839 0.4592 0.039(14) Uiso 1 1 calc R . . C20 C 0.3579(13) 0.9625(14) 0.5733(10) 0.047(4) Uani 1 1 d . . . H20A H 0.3881 0.8941 0.5674 0.039(14) Uiso 1 1 calc R . . H20B H 0.3308 0.9724 0.6401 0.039(14) Uiso 1 1 calc R . . H20C H 0.4176 1.0115 0.5608 0.039(14) Uiso 1 1 calc R . . H1 H -0.2109 0.8596 0.0946 0.02(6) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0188(2) 0.0176(2) 0.0163(2) 0.0011(2) 0.00136(14) 0.0006(2) O1 0.020(5) 0.036(5) 0.038(5) 0.013(5) -0.002(4) 0.001(4) O13 0.029(5) 0.031(5) 0.037(5) 0.006(4) -0.008(4) -0.010(4) O14 0.057(6) 0.035(6) 0.031(5) 0.001(4) 0.014(5) 0.010(5) O15 0.030(5) 0.031(5) 0.026(4) 0.008(4) -0.001(4) 0.005(4) N1 0.018(4) 0.018(5) 0.013(4) 0.000(3) 0.003(3) 0.001(4) N2 0.017(5) 0.022(5) 0.015(4) -0.006(4) 0.002(3) -0.001(4) N3 0.030(6) 0.031(6) 0.026(5) -0.003(5) 0.004(4) 0.006(5) C1 0.020(6) 0.012(5) 0.024(6) -0.005(4) 0.000(4) -0.005(4) C2 0.031(6) 0.016(5) 0.010(5) 0.000(4) 0.004(4) -0.002(5) C3 0.026(6) 0.023(6) 0.022(6) 0.000(5) 0.004(5) 0.001(5) C4 0.018(5) 0.022(6) 0.026(6) -0.001(5) -0.003(4) -0.001(5) C5 0.020(6) 0.034(7) 0.030(6) 0.009(5) 0.009(5) -0.002(5) C6 0.024(6) 0.030(7) 0.023(6) 0.007(5) 0.004(5) -0.002(5) C7 0.024(6) 0.020(6) 0.018(5) -0.003(5) 0.003(4) -0.002(5) C8 0.019(6) 0.028(6) 0.019(5) 0.001(5) 0.001(4) -0.002(5) C9 0.026(6) 0.022(6) 0.024(6) 0.006(5) 0.001(5) -0.003(5) C10 0.027(7) 0.023(6) 0.030(6) 0.006(5) 0.005(5) 0.006(5) C11 0.018(6) 0.020(6) 0.035(7) -0.001(5) -0.002(5) 0.005(5) C12 0.027(6) 0.027(6) 0.025(6) 0.008(5) 0.005(5) -0.003(5) C13 0.027(6) 0.019(6) 0.021(6) 0.005(5) -0.009(5) 0.001(5) C14 0.033(7) 0.026(7) 0.014(5) 0.002(5) 0.003(5) 0.000(5) C15 0.014(5) 0.027(6) 0.019(5) -0.003(5) 0.001(4) -0.005(5) C16 0.030(6) 0.020(6) 0.015(5) -0.001(4) -0.003(5) 0.000(5) C17 0.031(7) 0.031(7) 0.021(6) 0.003(5) 0.003(5) 0.000(6) C18 0.056(10) 0.037(8) 0.036(8) 0.000(7) 0.002(7) -0.012(8) C19 0.042(9) 0.051(10) 0.046(9) -0.008(7) 0.014(7) 0.011(7) C20 0.052(10) 0.063(11) 0.025(7) 0.001(7) -0.006(7) -0.003(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C15 1.937(12) . ? W1 C13 1.963(12) . ? W1 C14 1.987(11) . ? W1 C16 2.168(11) . ? W1 N1 2.228(9) . ? W1 N2 2.246(10) . ? O1 C4 1.359(13) . ? O1 H1 0.5758 . ? O13 C13 1.181(14) . ? O14 C14 1.155(14) . ? O15 C15 1.187(14) . ? N1 C7 1.287(14) . ? N1 C1 1.414(14) . ? N2 C12 1.328(15) . ? N2 C8 1.354(15) . ? N3 C16 1.145(14) . ? N3 C17 1.472(15) . ? C1 C6 1.395(15) . ? C1 C2 1.406(16) . ? C2 C3 1.362(16) . ? C2 H2 0.9300 . ? C3 C4 1.384(15) . ? C3 H3 0.9300 . ? C4 C5 1.401(17) . ? C4 H1 1.5938 . ? C5 C6 1.366(17) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.436(16) . ? C7 H7 0.9300 . ? C8 C9 1.399(17) . ? C9 C10 1.393(17) . ? C9 H9 0.9300 . ? C10 C11 1.383(17) . ? C10 H10 0.9300 . ? C11 C12 1.359(17) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C17 C19 1.510(19) . ? C17 C20 1.519(19) . ? C17 C18 1.529(19) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? 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 W1 C13 89.3(5) . . ? C15 W1 C14 88.2(5) . . ? C13 W1 C14 87.4(5) . . ? C15 W1 C16 94.4(5) . . ? C13 W1 C16 95.3(5) . . ? C14 W1 C16 176.3(5) . . ? C15 W1 N1 103.1(4) . . ? C13 W1 N1 167.5(4) . . ? C14 W1 N1 93.7(4) . . ? C16 W1 N1 83.1(4) . . ? C15 W1 N2 173.8(4) . . ? C13 W1 N2 95.5(4) . . ? C14 W1 N2 88.3(4) . . ? C16 W1 N2 88.9(4) . . ? N1 W1 N2 72.1(3) . . ? C4 O1 H1 103.4 . . ? C7 N1 C1 117.6(9) . . ? C7 N1 W1 117.7(8) . . ? C1 N1 W1 124.2(7) . . ? C12 N2 C8 117.7(10) . . ? C12 N2 W1 125.7(8) . . ? C8 N2 W1 116.0(7) . . ? C16 N3 C17 173.2(13) . . ? C6 C1 C2 117.6(11) . . ? C6 C1 N1 122.1(11) . . ? C2 C1 N1 120.3(9) . . ? C3 C2 C1 120.9(10) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 120.9(11) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? O1 C4 C3 124.2(11) . . ? O1 C4 C5 116.7(10) . . ? C3 C4 C5 119.1(11) . . ? O1 C4 H1 20.6 . . ? C3 C4 H1 104.6 . . ? C5 C4 H1 135.6 . . ? C6 C5 C4 119.8(10) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 121.7(11) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? N1 C7 C8 118.3(11) . . ? N1 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? N2 C8 C9 121.2(10) . . ? N2 C8 C7 115.3(11) . . ? C9 C8 C7 123.5(11) . . ? C10 C9 C8 119.9(11) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 117.3(11) . . ? C11 C10 H10 121.4 . . ? C9 C10 H10 121.4 . . ? C12 C11 C10 119.7(11) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.1 . . ? N2 C12 C11 124.2(12) . . ? N2 C12 H12 117.9 . . ? C11 C12 H12 117.9 . . ? O13 C13 W1 175.8(11) . . ? O14 C14 W1 178.1(12) . . ? O15 C15 W1 179.2(10) . . ? N3 C16 W1 173.9(11) . . ? N3 C17 C19 107.9(11) . . ? N3 C17 C20 107.1(11) . . ? C19 C17 C20 113.4(13) . . ? N3 C17 C18 105.8(11) . . ? C19 C17 C18 109.2(12) . . ? C20 C17 C18 113.0(12) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? 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 W1 N1 C7 175.1(8) . . . . ? C13 W1 N1 C7 -9(2) . . . . ? C14 W1 N1 C7 86.1(8) . . . . ? C16 W1 N1 C7 -92.0(8) . . . . ? N2 W1 N1 C7 -0.9(7) . . . . ? C15 W1 N1 C1 -12.5(9) . . . . ? C13 W1 N1 C1 163.9(18) . . . . ? C14 W1 N1 C1 -101.5(8) . . . . ? C16 W1 N1 C1 80.5(8) . . . . ? N2 W1 N1 C1 171.6(9) . . . . ? C15 W1 N2 C12 136(3) . . . . ? C13 W1 N2 C12 -5.3(10) . . . . ? C14 W1 N2 C12 81.9(10) . . . . ? C16 W1 N2 C12 -100.6(9) . . . . ? N1 W1 N2 C12 176.3(10) . . . . ? C15 W1 N2 C8 -35(4) . . . . ? C13 W1 N2 C8 -176.7(8) . . . . ? C14 W1 N2 C8 -89.4(8) . . . . ? C16 W1 N2 C8 88.1(8) . . . . ? N1 W1 N2 C8 5.0(7) . . . . ? C7 N1 C1 C6 44.0(15) . . . . ? W1 N1 C1 C6 -128.5(10) . . . . ? C7 N1 C1 C2 -138.3(11) . . . . ? W1 N1 C1 C2 49.3(13) . . . . ? C6 C1 C2 C3 -2.0(17) . . . . ? N1 C1 C2 C3 -179.8(10) . . . . ? C1 C2 C3 C4 2.7(18) . . . . ? C2 C3 C4 O1 177.5(11) . . . . ? C2 C3 C4 C5 -1.9(18) . . . . ? O1 C4 C5 C6 -179.0(11) . . . . ? C3 C4 C5 C6 0.5(19) . . . . ? C4 C5 C6 C1 0(2) . . . . ? C2 C1 C6 C5 0.6(18) . . . . ? N1 C1 C6 C5 178.4(11) . . . . ? C1 N1 C7 C8 -176.1(9) . . . . ? W1 N1 C7 C8 -3.2(13) . . . . ? C12 N2 C8 C9 -1.9(16) . . . . ? W1 N2 C8 C9 170.2(8) . . . . ? C12 N2 C8 C7 179.7(10) . . . . ? W1 N2 C8 C7 -8.3(12) . . . . ? N1 C7 C8 N2 7.7(15) . . . . ? N1 C7 C8 C9 -170.7(11) . . . . ? N2 C8 C9 C10 1.7(17) . . . . ? C7 C8 C9 C10 -179.9(11) . . . . ? C8 C9 C10 C11 0.4(17) . . . . ? C9 C10 C11 C12 -2.3(18) . . . . ? C8 N2 C12 C11 -0.2(17) . . . . ? W1 N2 C12 C11 -171.4(9) . . . . ? C10 C11 C12 N2 2.3(19) . . . . ? C15 W1 C13 O13 -135(13) . . . . ? C14 W1 C13 O13 -46(13) . . . . ? C16 W1 C13 O13 131(13) . . . . ? N1 W1 C13 O13 49(14) . . . . ? N2 W1 C13 O13 42(13) . . . . ? C15 W1 C14 O14 152(34) . . . . ? C13 W1 C14 O14 62(34) . . . . ? C16 W1 C14 O14 -74(37) . . . . ? N1 W1 C14 O14 -105(34) . . . . ? N2 W1 C14 O14 -33(34) . . . . ? C13 W1 C15 O15 128(68) . . . . ? C14 W1 C15 O15 40(68) . . . . ? C16 W1 C15 O15 -137(68) . . . . ? N1 W1 C15 O15 -53(68) . . . . ? N2 W1 C15 O15 -14(70) . . . . ? C17 N3 C16 W1 35(19) . . . . ? C15 W1 C16 N3 103(10) . . . . ? C13 W1 C16 N3 -167(10) . . . . ? C14 W1 C16 N3 -31(15) . . . . ? N1 W1 C16 N3 1(10) . . . . ? N2 W1 C16 N3 -72(10) . . . . ? C16 N3 C17 C19 -157(10) . . . . ? C16 N3 C17 C20 81(11) . . . . ? C16 N3 C17 C18 -40(11) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 5.328 _refine_diff_density_min -2.407 _refine_diff_density_rms 0.332 #===END