#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_contact_author 'Prof H W Roesky' _publ_contact_author_address ; Prof H W Roesky Institut fur Anorganische Chemie der Georg-August-Universitat Gottingen Tammannstr. 4 37077 Gottingen GERMANY ; _publ_contact_author_email 'HROESKY@GWDG.DE' _publ_requested_journal 'J.Chem.Soc.,Dalton Transactions' _publ_contact_letter ; ? ; #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Acetylacetonatodifluorooxometalates of vanadium and molybdenum: synthesis and crystal structures ; loop_ _publ_author_name _publ_author_name 'Andreas Stasch' ; Institut fur Anorganische Chemie Universitat Gottingen Tammannstr. 4 37077 Gottingen Germany ; ' Herbert W. Roesky' ; Institut fur Anorganische Chemie Universitat G\"ottingen Tammannstr. 4 37077 Gottingen Germany ; 'Hans-Georg Schmidt' ; Institut fur Anorganische Chemie Universitat Gottingen Tammannstr. 4 37077 Gottingen Germany ; 'Mathias Noltemeyer' ; Institut fur Anorganische Chemie Universitat G\"ottingen Tammannstr. 4 37077 Gottingen Germany ; ' Mark Schormann' ; Institut fur Anorganische Chemie Universitat G\"ottingen Tammannstr. 4 37077 Gottingen Germany ; 'Jorg Prust' ; Institut fur Anorganische Chemie Universitat Gottingen Tammannstr. 4 37077 Gottingen Germany ; #============================================================================== # 3. TEXT _publ_section_comment ; The compounds 1 and 2 were determined by Xray Structure Analysis. ; _publ_section_experimental ; Programs were developed by the following authors : ; _publ_section_references ; Clegg, W. (1981). Acta Cryst. A37, 22-28. Langhoff, H. (1986). DIF4 rev 6.2 , STOE & CIE, Darmstadt. Sheldrick, G.M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G.M. (1993). SHELXL-97, Program for crystal structure refinement, University of G\"ottingen. Sheldrick, G.M. (1992). SHELXTL , Siemens Analytical Instruments, Madison. ; #============================================================================== data_roe902x _database_code_CSD 154686 _audit_creation_method SHELXL #_chemical_name_systematic 'compound 1' _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C13 H27 F2 N O3 V' _chemical_formula_weight 334.30 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.060(2) _cell_length_b 12.6046(11) _cell_length_c 20.467(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3369.2(9) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12 _exptl_crystal_description blocks _exptl_crystal_colour none _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method ? _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.614 _exptl_absorpt_correction_type 'azimuthal scans' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'STOE AED2 four circle diffractometer' _diffrn_measurement_method 'profile fitted theta omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '90 min' _diffrn_standards_decay_% none _diffrn_reflns_number 3277 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2976 _reflns_number_observed 2267 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STOE DIF4' _computing_cell_refinement 'STOE DIF4' _computing_data_reduction 'STOE REDU4' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 11 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+2.7401P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2965 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_obs 0.0402 _refine_ls_wR_factor_all 0.1198 _refine_ls_wR_factor_obs 0.0933 _refine_ls_goodness_of_fit_all 1.082 _refine_ls_goodness_of_fit_obs 1.062 _refine_ls_restrained_S_all 1.181 _refine_ls_restrained_S_obs 1.062 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group V1 V -0.00128(3) -0.00570(3) 0.36316(2) 0.0237(2) Uani 1 d . . F1 F -0.14246(11) -0.02023(12) 0.34944(8) 0.0323(4) Uani 1 d . . F2 F 0.00935(11) -0.15256(12) 0.35208(8) 0.0331(4) Uani 1 d . . O1 O -0.04098(15) 0.11595(15) 0.42076(9) 0.0319(5) Uani 1 d . . O2 O 0.12200(14) -0.02246(15) 0.42106(9) 0.0325(5) Uani 1 d . . O3 O 0.0445(2) 0.0512(2) 0.29997(9) 0.0369(5) Uani 1 d . . C1 C -0.0446(3) 0.2518(3) 0.4998(2) 0.0467(8) Uani 1 d . . H1A H -0.1191(3) 0.2452(9) 0.4953(10) 0.070 Uiso 1 calc R . H1B H -0.0215(13) 0.3164(3) 0.4777(7) 0.070 Uiso 1 calc R . H1C H -0.0265(14) 0.2554(10) 0.5462(3) 0.070 Uiso 1 calc R . C2 C 0.0062(2) 0.1570(2) 0.46927(13) 0.0299(6) Uani 1 d . . C3 C 0.0974(2) 0.1194(2) 0.49501(13) 0.0334(7) Uani 1 d . . H3B H 0.1252(2) 0.1548(2) 0.53193(13) 0.040 Uiso 1 calc R . C4 C 0.1507(2) 0.0327(2) 0.46996(13) 0.0295(6) Uani 1 d . . C5 C 0.2492(2) -0.0013(3) 0.50145(14) 0.0402(7) Uani 1 d . . H5A H 0.2517(7) -0.0789(3) 0.5036(9) 0.060 Uiso 1 calc R . H5B H 0.2531(8) 0.0281(14) 0.5457(4) 0.060 Uiso 1 calc R . H5C H 0.3071(2) 0.0247(14) 0.4756(6) 0.060 Uiso 1 calc R . N1 N 0.2234(2) -0.2625(2) 0.25008(10) 0.0235(5) Uani 1 d . . C6 C 0.2091(2) -0.3747(2) 0.27602(13) 0.0280(6) Uani 1 d . . H6A H 0.1931(2) -0.4220(2) 0.23875(13) 0.034 Uiso 1 calc R . H6B H 0.2748(2) -0.3989(2) 0.29503(13) 0.034 Uiso 1 calc R . C61 C 0.1261(2) -0.3876(2) 0.32703(14) 0.0391(7) Uani 1 d . . H61A H 0.1224(11) -0.4621(4) 0.3406(7) 0.059 Uiso 1 calc R . H61B H 0.0602(3) -0.3658(15) 0.3086(3) 0.059 Uiso 1 calc R . H61C H 0.1421(8) -0.3432(12) 0.3650(4) 0.059 Uiso 1 calc R . C7 C 0.3174(2) -0.2607(2) 0.20623(13) 0.0296(6) Uani 1 d . . H7A H 0.3338(2) -0.1859(2) 0.19581(13) 0.036 Uiso 1 calc R . H7B H 0.3760(2) -0.2902(2) 0.23097(13) 0.036 Uiso 1 calc R . C71 C 0.3073(2) -0.3215(2) 0.14282(14) 0.0397(7) Uani 1 d . . H71A H 0.3728(5) -0.3204(14) 0.1195(5) 0.060 Uiso 1 calc R . H71B H 0.2544(11) -0.2884(10) 0.1156(4) 0.060 Uiso 1 calc R . H71C H 0.2880(15) -0.3951(5) 0.15223(15) 0.060 Uiso 1 calc R . C8 C 0.2395(2) -0.1837(2) 0.30505(13) 0.0299(6) Uani 1 d . . H8A H 0.1756(2) -0.1792(2) 0.33095(13) 0.036 Uiso 1 calc R . H8B H 0.2522(2) -0.1129(2) 0.28580(13) 0.036 Uiso 1 calc R . C81 C 0.3272(2) -0.2104(3) 0.3507(2) 0.0464(8) Uani 1 d . . H81A H 0.3334(11) -0.1548(10) 0.3840(7) 0.070 Uiso 1 calc R . H81B H 0.3910(4) -0.2148(18) 0.3257(2) 0.070 Uiso 1 calc R . H81C H 0.3138(9) -0.2786(9) 0.3720(8) 0.070 Uiso 1 calc R . C9 C 0.1270(2) -0.2317(2) 0.21302(14) 0.0288(6) Uani 1 d . . H9A H 0.1138(2) -0.2860(2) 0.17910(14) 0.035 Uiso 1 calc R . H9B H 0.0685(2) -0.2330(2) 0.24379(14) 0.035 Uiso 1 calc R . C91 C 0.1305(2) -0.1239(2) 0.18045(14) 0.0365(7) Uani 1 d . . H91A H 0.0714(8) -0.1161(6) 0.1514(7) 0.055 Uiso 1 calc R . H91B H 0.1938(7) -0.1175(6) 0.1550(8) 0.055 Uiso 1 calc R . H91C H 0.1287(15) -0.0683(2) 0.21391(15) 0.055 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0230(2) 0.0224(2) 0.0256(3) -0.0027(2) -0.0009(2) -0.0006(2) F1 0.0244(8) 0.0298(9) 0.0427(9) -0.0042(7) -0.0037(7) 0.0006(7) F2 0.0302(9) 0.0246(8) 0.0446(9) -0.0082(7) -0.0020(7) 0.0011(7) O1 0.0365(11) 0.0272(10) 0.0321(10) -0.0060(9) -0.0034(9) 0.0044(9) O2 0.0286(10) 0.0354(11) 0.0335(11) -0.0085(9) -0.0053(8) 0.0028(9) O3 0.0395(11) 0.0378(12) 0.0335(11) -0.0010(9) 0.0029(9) -0.0079(10) C1 0.069(2) 0.032(2) 0.039(2) -0.0083(13) -0.004(2) 0.012(2) C2 0.042(2) 0.0228(14) 0.0251(13) -0.0003(11) 0.0029(13) -0.0045(13) C3 0.042(2) 0.033(2) 0.0249(14) -0.0047(13) -0.0043(13) -0.0066(14) C4 0.0298(15) 0.034(2) 0.0243(14) 0.0038(13) -0.0006(12) -0.0083(13) C5 0.0320(15) 0.055(2) 0.0334(15) -0.0029(14) -0.0053(14) 0.0001(14) N1 0.0224(11) 0.0188(10) 0.0293(11) -0.0007(10) 0.0011(9) -0.0017(9) C6 0.0326(14) 0.0183(13) 0.0331(14) 0.0010(11) 0.0020(12) 0.0016(12) C61 0.046(2) 0.032(2) 0.040(2) 0.0080(14) 0.0107(15) 0.0011(14) C7 0.0252(14) 0.0271(15) 0.036(2) 0.0014(12) 0.0067(12) -0.0033(12) C71 0.046(2) 0.038(2) 0.036(2) -0.0023(14) 0.0147(14) -0.0040(14) C8 0.0317(15) 0.0226(14) 0.0353(15) -0.0060(12) -0.0029(13) 0.0008(12) C81 0.047(2) 0.046(2) 0.046(2) -0.014(2) -0.017(2) 0.004(2) C9 0.0231(13) 0.0298(15) 0.0334(15) 0.0026(12) -0.0045(12) -0.0015(12) C91 0.036(2) 0.035(2) 0.039(2) 0.0086(14) -0.0053(14) 0.0009(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 V1 O3 1.595(2) . ? V1 F2 1.870(2) . ? V1 F1 1.874(2) . ? V1 O1 2.003(2) . ? V1 O2 2.010(2) . ? O1 C2 1.278(3) . ? O2 C4 1.275(3) . ? C1 C2 1.502(4) . ? C2 C3 1.386(4) . ? C3 C4 1.394(4) . ? C4 C5 1.501(4) . ? N1 C8 1.515(3) . ? N1 C9 1.521(3) . ? N1 C7 1.521(3) . ? N1 C6 1.522(3) . ? C6 C61 1.513(4) . ? C7 C71 1.513(4) . ? C8 C81 1.516(4) . ? C9 C91 1.515(4) . ? 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 O3 V1 F2 108.61(9) . . ? O3 V1 F1 106.93(9) . . ? F2 V1 F1 87.60(7) . . ? O3 V1 O1 103.30(9) . . ? F2 V1 O1 148.05(8) . . ? F1 V1 O1 84.74(7) . . ? O3 V1 O2 103.00(9) . . ? F2 V1 O2 84.72(7) . . ? F1 V1 O2 150.00(8) . . ? O1 V1 O2 86.60(8) . . ? C2 O1 V1 130.0(2) . . ? C4 O2 V1 129.9(2) . . ? O1 C2 C3 124.8(3) . . ? O1 C2 C1 115.6(3) . . ? C3 C2 C1 119.6(3) . . ? C2 C3 C4 123.9(3) . . ? O2 C4 C3 124.7(3) . . ? O2 C4 C5 115.7(3) . . ? C3 C4 C5 119.6(3) . . ? C8 N1 C9 108.5(2) . . ? C8 N1 C7 108.5(2) . . ? C9 N1 C7 111.7(2) . . ? C8 N1 C6 111.5(2) . . ? C9 N1 C6 108.0(2) . . ? C7 N1 C6 108.6(2) . . ? C61 C6 N1 115.3(2) . . ? C71 C7 N1 115.3(2) . . ? N1 C8 C81 114.7(2) . . ? C91 C9 N1 115.1(2) . . ? _refine_diff_density_max 0.297 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.055 data_roe906 _database_code_CSD 154687 _audit_creation_method SHELXL-97 #_chemical_name_systematic 'compound 2' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H27 F2 Mo N O4' _chemical_formula_weight 395.30 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 15.718(3) _cell_length_b 8.1649(10) _cell_length_c 13.421(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.644(15) _cell_angle_gamma 90.00 _cell_volume 1702.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12 _exptl_crystal_description blocks _exptl_crystal_colour none _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.80 _exptl_crystal_size_min 0.80 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.803 _exptl_absorpt_correction_type 'azimuthal scans' _exptl_absorpt_correction_T_min 0.5006 _exptl_absorpt_correction_T_max 0.5659 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE AED2 four circle diffractometer' _diffrn_measurement_method 'profile fitted theta omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '90 min' _diffrn_standards_decay_% none _diffrn_reflns_number 2381 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0056 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2377 _reflns_number_gt 2364 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE DIF4' _computing_cell_refinement 'STOE DIF4' _computing_data_reduction 'STOE REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+3.8000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0241(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 2377 _refine_ls_number_parameters 197 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 3.274 _refine_ls_shift/su_mean 0.098 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 0.22532(8) 1.20813(4) 0.23911(11) 0.0296(2) Uani 1 1 d . . . F1 F 0.1135(4) 1.1572(11) 0.1653(5) 0.0511(16) Uani 1 1 d . . . O1 O 0.1894(5) 1.0031(11) 0.3283(5) 0.038(2) Uani 1 1 d . . . N1 N 0.4720(6) 0.7636(17) 0.4900(8) 0.0233(13) Uani 1 1 d . . . C1 C 0.1950(6) 0.8453(15) 0.3174(9) 0.037(3) Uani 1 1 d . . . F2 F 0.3355(3) 1.1665(10) 0.3151(5) 0.0451(16) Uani 1 1 d . . . O2 O 0.2600(5) 1.0037(10) 0.1510(6) 0.040(2) Uani 1 1 d . . . C2 C 0.2278(11) 0.7686(6) 0.2379(15) 0.0328(12) Uani 1 1 d . . . H2A H 0.2315 0.6525 0.2386 0.039 Uiso 1 1 calc R . . O3 O 0.1879(5) 1.3288(15) 0.3277(6) 0.047(2) Uani 1 1 d . . . C3 C 0.2555(5) 0.8520(15) 0.1579(7) 0.028(2) Uani 1 1 d . . . O4 O 0.2565(5) 1.3429(14) 0.1574(6) 0.0409(16) Uani 1 1 d . . . C4 C 0.2861(9) 0.7561(16) 0.0755(13) 0.063(4) Uani 1 1 d . . . H4B H 0.2711 0.8143 0.0114 0.095 Uiso 1 1 calc R . . H4C H 0.2587 0.6480 0.0707 0.095 Uiso 1 1 calc R . . H4D H 0.3488 0.7430 0.0903 0.095 Uiso 1 1 calc R . . C5 C 0.1661(7) 0.7449(15) 0.4009(9) 0.044(3) Uani 1 1 d . . . H5A H 0.1094 0.7829 0.4130 0.066 Uiso 1 1 calc R . . H5B H 0.2077 0.7575 0.4626 0.066 Uiso 1 1 calc R . . H5C H 0.1625 0.6293 0.3812 0.066 Uiso 1 1 calc R . . C11 C 0.5085(6) 0.5842(9) 0.4588(7) 0.068(2) Uani 1 1 d . . . H11A H 0.5398 0.5933 0.4003 0.082 Uiso 1 1 calc R . . H11B H 0.5465 0.5334 0.5160 0.082 Uiso 1 1 calc R . . C12 C 0.4215(17) 0.4851(19) 0.4311(14) 0.184(12) Uani 1 1 d . . . H12A H 0.4235 0.4212 0.3697 0.276 Uiso 1 1 calc R . . H12B H 0.3730 0.5619 0.4198 0.276 Uiso 1 1 calc R . . H12C H 0.4141 0.4111 0.4866 0.276 Uiso 1 1 calc R . . C13 C 0.4260(4) 0.7383(10) 0.5716(6) 0.0415(14) Uani 1 1 d . . . H13A H 0.3760 0.6673 0.5479 0.050 Uiso 1 1 calc R . . H13B H 0.4032 0.8453 0.5900 0.050 Uiso 1 1 calc R . . C14 C 0.4774(7) 0.6588(17) 0.6707(8) 0.053(3) Uani 1 1 d . . . H10A H 0.4366 0.6132 0.7118 0.080 Uiso 1 1 calc R . . H10B H 0.5126 0.7429 0.7094 0.080 Uiso 1 1 calc R . . H10C H 0.5147 0.5713 0.6522 0.080 Uiso 1 1 calc R . . C15 C 0.5599(6) 0.8478(15) 0.5192(7) 0.076(3) Uani 1 1 d . . . H15A H 0.5893 0.8626 0.4595 0.092 Uiso 1 1 calc R . . H15B H 0.5975 0.7832 0.5705 0.092 Uiso 1 1 calc R . . C16 C 0.5341(14) 1.0337(17) 0.5671(14) 0.122(6) Uani 1 1 d . . . H16A H 0.5855 1.1032 0.5784 0.183 Uiso 1 1 calc R . . H16B H 0.5125 1.0165 0.6311 0.183 Uiso 1 1 calc R . . H16C H 0.4896 1.0873 0.5191 0.183 Uiso 1 1 calc R . . C17 C 0.4252(4) 0.8304(12) 0.4006(6) 0.0535(18) Uani 1 1 d . . . H17A H 0.4043 0.9402 0.4167 0.064 Uiso 1 1 calc R . . H17B H 0.3740 0.7608 0.3803 0.064 Uiso 1 1 calc R . . C18 C 0.4744(8) 0.848(2) 0.3071(9) 0.073(4) Uani 1 1 d . . . H18A H 0.4351 0.8914 0.2495 0.110 Uiso 1 1 calc R . . H18B H 0.4957 0.7406 0.2897 0.110 Uiso 1 1 calc R . . H18C H 0.5230 0.9233 0.3239 0.110 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0319(2) 0.0229(3) 0.0343(3) -0.0004(4) 0.00573(16) 0.0003(3) F1 0.050(4) 0.055(3) 0.045(4) -0.011(4) -0.006(3) -0.007(4) O1 0.042(4) 0.045(5) 0.030(4) 0.010(4) 0.016(3) -0.003(3) N1 0.0231(18) 0.018(4) 0.029(2) -0.0010(19) 0.0031(15) 0.0070(17) C1 0.038(5) 0.023(5) 0.048(7) 0.007(5) 0.003(5) -0.007(5) F2 0.026(3) 0.047(3) 0.062(5) -0.013(4) 0.001(3) -0.001(3) O2 0.057(5) 0.019(4) 0.047(5) 0.008(3) 0.020(4) 0.000(3) C2 0.033(2) 0.028(2) 0.037(3) 0.013(7) 0.001(2) 0.005(5) O3 0.056(4) 0.036(4) 0.053(5) -0.008(4) 0.023(3) 0.005(4) C3 0.023(4) 0.040(6) 0.022(5) -0.003(5) 0.000(4) 0.001(5) O4 0.054(4) 0.023(3) 0.046(4) 0.001(3) 0.011(3) 0.000(3) C4 0.077(10) 0.042(5) 0.075(11) -0.026(8) 0.026(9) -0.006(7) C5 0.059(8) 0.044(4) 0.030(6) 0.005(6) 0.014(6) -0.016(6) C11 0.098(6) 0.043(4) 0.072(6) 0.011(4) 0.040(5) 0.029(4) C12 0.40(3) 0.090(9) 0.084(9) -0.068(8) 0.101(14) -0.173(15) C13 0.032(3) 0.057(4) 0.038(4) 0.005(3) 0.013(3) 0.004(3) C14 0.050(5) 0.074(6) 0.033(5) 0.028(6) -0.004(4) -0.006(6) C15 0.054(4) 0.137(8) 0.039(4) -0.013(5) 0.010(3) -0.055(5) C16 0.208(16) 0.068(8) 0.098(11) -0.054(7) 0.049(9) -0.077(9) C17 0.033(3) 0.085(5) 0.044(4) 0.019(4) 0.009(3) 0.017(3) C18 0.063(7) 0.127(11) 0.039(6) 0.014(9) 0.036(6) 0.023(9) _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 O4 1.678(10) . ? Mo1 O3 1.714(10) . ? Mo1 F2 1.904(6) . ? Mo1 F1 1.929(6) . ? Mo1 O2 2.162(8) . ? Mo1 O1 2.182(8) . ? O1 C1 1.301(18) . ? N1 C13 1.416(13) . ? N1 C17 1.419(13) . ? N1 C15 1.540(13) . ? N1 C11 1.650(13) . ? C1 C2 1.40(2) . ? C1 C5 1.512(15) . ? O2 C3 1.245(16) . ? C2 C3 1.40(2) . ? C3 C4 1.493(16) . ? C11 C12 1.58(2) . ? C13 C14 1.587(12) . ? C15 C16 1.721(17) . ? C17 C18 1.577(12) . ? 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 O4 Mo1 O3 103.9(2) . . ? O4 Mo1 F2 97.8(4) . . ? O3 Mo1 F2 96.3(4) . . ? O4 Mo1 F1 98.0(4) . . ? O3 Mo1 F1 95.7(4) . . ? F2 Mo1 F1 157.24(15) . . ? O4 Mo1 O2 91.5(4) . . ? O3 Mo1 O2 164.5(4) . . ? F2 Mo1 O2 82.6(3) . . ? F1 Mo1 O2 80.7(3) . . ? O4 Mo1 O1 170.8(4) . . ? O3 Mo1 O1 85.2(4) . . ? F2 Mo1 O1 81.9(3) . . ? F1 Mo1 O1 79.9(3) . . ? O2 Mo1 O1 79.33(12) . . ? C1 O1 Mo1 132.1(8) . . ? C13 N1 C17 116.8(7) . . ? C13 N1 C15 114.3(9) . . ? C17 N1 C15 112.1(11) . . ? C13 N1 C11 107.7(10) . . ? C17 N1 C11 106.4(9) . . ? C15 N1 C11 97.4(7) . . ? O1 C1 C2 124.6(11) . . ? O1 C1 C5 114.9(11) . . ? C2 C1 C5 120.5(11) . . ? C3 O2 Mo1 134.9(8) . . ? C3 C2 C1 124.1(4) . . ? O2 C3 C2 124.8(11) . . ? O2 C3 C4 116.0(11) . . ? C2 C3 C4 119.1(12) . . ? C12 C11 N1 101.1(10) . . ? N1 C13 C14 117.0(7) . . ? N1 C15 C16 103.6(10) . . ? N1 C17 C18 117.0(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.499 _refine_diff_density_min -0.998 _refine_diff_density_rms 0.114 #eof