# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email appell@uni-koeln.de loop_ _publ_author_name 'L. Appel' 'R. Fiz' 'W. Tyrra' 'S. Mathur' _publ_contact_author_name 'Linus Appel' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 809950' #TrackingRef 'ap001.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H41 Cl N Nb O4' _chemical_formula_sum 'C21 H41 Cl N Nb O4' _chemical_formula_weight 499.91 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' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 16.5068(13) _cell_length_b 9.9031(5) _cell_length_c 17.1689(14) _cell_angle_alpha 90.00 _cell_angle_beta 105.610(6) _cell_angle_gamma 90.00 _cell_volume 2703.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 44119 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 29.61 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.566 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.8344 _exptl_absorpt_correction_T_max 0.9489 _exptl_absorpt_process_details ; The absorption correction (X-RED; Stoe & Cie, 2001) was performed after optimizing the crytal shape using X-SHAPE (Soe & Cie, 1999). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(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 'IPDS II (Stoe & Cie)' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 14547 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 29.61 _reflns_number_total 7565 _reflns_number_gt 5614 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _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^)+(0.0842P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0117(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7565 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1224 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.016 _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 Nb1 Nb 0.743442(12) 0.07745(2) 0.295098(12) 0.02746(8) Uani 1 1 d . . . Cl1 Cl 0.61825(4) 0.11069(7) 0.35321(4) 0.03593(14) Uani 1 1 d . . . O1 O 0.77786(12) 0.24981(19) 0.33876(11) 0.0393(4) Uani 1 1 d . . . O2 O 0.82689(12) 0.0710(2) 0.23921(12) 0.0410(4) Uani 1 1 d . . . N1 N 0.66270(13) 0.2059(2) 0.18558(12) 0.0330(4) Uani 1 1 d . . . O3 O 0.67977(11) -0.06291(18) 0.23377(11) 0.0347(4) Uani 1 1 d . . . O4 O 0.79637(11) -0.0248(2) 0.38545(11) 0.0373(4) Uani 1 1 d . . . C1 C 0.60765(17) 0.3018(3) 0.19195(16) 0.0386(6) Uani 1 1 d . . . H1 H 0.6004 0.3200 0.2428 0.046 Uiso 1 1 calc R . . C2 C 0.56096(19) 0.3752(3) 0.12652(18) 0.0468(7) Uani 1 1 d . . . H2 H 0.5227 0.4402 0.1332 0.056 Uiso 1 1 calc R . . C3 C 0.5726(2) 0.3494(4) 0.05077(18) 0.0524(8) Uani 1 1 d . . . H3 H 0.5430 0.3980 0.0057 0.063 Uiso 1 1 calc R . . C4 C 0.6288(2) 0.2506(4) 0.04356(17) 0.0496(7) Uani 1 1 d . . . H4 H 0.6376 0.2314 -0.0065 0.059 Uiso 1 1 calc R . . C5 C 0.67200(17) 0.1805(3) 0.11170(15) 0.0409(6) Uani 1 1 d . . . H5 H 0.7091 0.1128 0.1061 0.049 Uiso 1 1 calc R . . C6 C 0.61227(18) -0.1521(3) 0.19826(17) 0.0402(6) Uani 1 1 d . . . C7 C 0.6370(2) -0.2285(4) 0.1310(2) 0.0602(9) Uani 1 1 d . . . H7A H 0.6432 -0.1659 0.0903 0.090 Uiso 1 1 calc R . . H7B H 0.5942 -0.2932 0.1074 0.090 Uiso 1 1 calc R . . H7C H 0.6894 -0.2745 0.1531 0.090 Uiso 1 1 calc R . . C8 C 0.53166(19) -0.0708(3) 0.1643(2) 0.0486(7) Uani 1 1 d . . . H8A H 0.5395 -0.0100 0.1234 0.073 Uiso 1 1 calc R . . H8B H 0.5187 -0.0201 0.2071 0.073 Uiso 1 1 calc R . . H8C H 0.4861 -0.1313 0.1412 0.073 Uiso 1 1 calc R . . C9 C 0.6023(2) -0.2494(3) 0.2632(2) 0.0517(7) Uani 1 1 d . . . H9A H 0.5867 -0.2002 0.3051 0.078 Uiso 1 1 calc R . . H9B H 0.6546 -0.2954 0.2856 0.078 Uiso 1 1 calc R . . H9C H 0.5593 -0.3141 0.2399 0.078 Uiso 1 1 calc R . . C10 C 0.81933(19) -0.0748(3) 0.46624(17) 0.0422(6) Uani 1 1 d . . . C11 C 0.7459(2) -0.1541(4) 0.4789(2) 0.0657(10) Uani 1 1 d . . . H11A H 0.6985 -0.0952 0.4731 0.099 Uiso 1 1 calc R . . H11B H 0.7609 -0.1927 0.5321 0.099 Uiso 1 1 calc R . . H11C H 0.7317 -0.2250 0.4394 0.099 Uiso 1 1 calc R . . C12 C 0.8388(3) 0.0463(5) 0.5230(2) 0.0755(12) Uani 1 1 d . . . H12A H 0.8856 0.0952 0.5139 0.113 Uiso 1 1 calc R . . H12B H 0.8524 0.0157 0.5780 0.113 Uiso 1 1 calc R . . H12C H 0.7905 0.1044 0.5127 0.113 Uiso 1 1 calc R . . C13 C 0.8959(2) -0.1642(4) 0.4748(2) 0.0639(10) Uani 1 1 d . . . H13A H 0.9416 -0.1112 0.4665 0.096 Uiso 1 1 calc R . . H13B H 0.8827 -0.2351 0.4353 0.096 Uiso 1 1 calc R . . H13C H 0.9119 -0.2028 0.5280 0.096 Uiso 1 1 calc R . . C14 C 0.80683(18) 0.3824(3) 0.36040(18) 0.0399(6) Uani 1 1 d . . . C15 C 0.7514(3) 0.4434(4) 0.4092(3) 0.0686(11) Uani 1 1 d . . . H15A H 0.7561 0.3905 0.4571 0.103 Uiso 1 1 calc R . . H15B H 0.6940 0.4440 0.3771 0.103 Uiso 1 1 calc R . . H15C H 0.7693 0.5343 0.4242 0.103 Uiso 1 1 calc R . . C16 C 0.8975(2) 0.3732(4) 0.4110(2) 0.0620(9) Uani 1 1 d . . . H16A H 0.9002 0.3222 0.4592 0.093 Uiso 1 1 calc R . . H16B H 0.9191 0.4624 0.4255 0.093 Uiso 1 1 calc R . . H16C H 0.9307 0.3292 0.3803 0.093 Uiso 1 1 calc R . . C17 C 0.8015(3) 0.4627(4) 0.2841(2) 0.0641(9) Uani 1 1 d . . . H17A H 0.7440 0.4679 0.2525 0.096 Uiso 1 1 calc R . . H17B H 0.8344 0.4189 0.2530 0.096 Uiso 1 1 calc R . . H17C H 0.8229 0.5521 0.2982 0.096 Uiso 1 1 calc R . . C18 C 0.89783(17) 0.0265(4) 0.21638(18) 0.0452(6) Uani 1 1 d . . . C19 C 0.9704(2) 0.0176(7) 0.2885(3) 0.0864(15) Uani 1 1 d . . . H19A H 0.9820 0.1052 0.3128 0.130 Uiso 1 1 calc R . . H19B H 1.0187 -0.0141 0.2728 0.130 Uiso 1 1 calc R . . H19C H 0.9577 -0.0443 0.3266 0.130 Uiso 1 1 calc R . . C20 C 0.9159(3) 0.1295(8) 0.1582(4) 0.128(3) Uani 1 1 d . . . H20A H 0.8686 0.1351 0.1113 0.192 Uiso 1 1 calc R . . H20B H 0.9649 0.1025 0.1421 0.192 Uiso 1 1 calc R . . H20C H 0.9256 0.2160 0.1842 0.192 Uiso 1 1 calc R . . C21 C 0.8761(4) -0.1058(8) 0.1753(6) 0.163(4) Uani 1 1 d . . . H21A H 0.8287 -0.0950 0.1290 0.245 Uiso 1 1 calc R . . H21B H 0.8623 -0.1691 0.2121 0.245 Uiso 1 1 calc R . . H21C H 0.9233 -0.1389 0.1583 0.245 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 Nb1 0.02622(11) 0.02948(13) 0.02672(12) 0.00110(8) 0.00720(7) 0.00103(8) Cl1 0.0347(3) 0.0437(3) 0.0320(3) 0.0004(2) 0.0134(2) 0.0040(2) O1 0.0422(10) 0.0317(10) 0.0412(10) -0.0013(8) 0.0065(8) -0.0068(8) O2 0.0313(9) 0.0546(12) 0.0417(10) 0.0092(8) 0.0179(8) 0.0089(8) N1 0.0305(9) 0.0382(11) 0.0301(9) 0.0022(8) 0.0078(8) 0.0025(8) O3 0.0342(9) 0.0337(9) 0.0348(9) -0.0048(7) 0.0068(7) -0.0018(7) O4 0.0366(9) 0.0406(10) 0.0341(9) 0.0078(8) 0.0083(7) 0.0040(8) C1 0.0416(13) 0.0400(14) 0.0366(12) 0.0038(11) 0.0145(10) 0.0077(11) C2 0.0461(15) 0.0493(16) 0.0475(15) 0.0098(13) 0.0168(13) 0.0173(13) C3 0.0552(18) 0.061(2) 0.0400(14) 0.0169(14) 0.0110(13) 0.0177(15) C4 0.0548(17) 0.064(2) 0.0309(12) 0.0079(13) 0.0128(12) 0.0166(15) C5 0.0404(13) 0.0507(16) 0.0322(12) 0.0033(11) 0.0107(10) 0.0101(12) C6 0.0390(13) 0.0384(15) 0.0419(14) -0.0084(11) 0.0088(11) -0.0041(11) C7 0.0612(19) 0.065(2) 0.0551(18) -0.0291(17) 0.0158(15) -0.0125(17) C8 0.0372(14) 0.0528(18) 0.0506(16) -0.0019(14) 0.0026(12) -0.0030(12) C9 0.0472(16) 0.0442(17) 0.0624(19) 0.0039(14) 0.0124(14) -0.0052(13) C10 0.0418(14) 0.0480(16) 0.0331(12) 0.0094(11) 0.0038(10) 0.0037(12) C11 0.058(2) 0.075(3) 0.066(2) 0.034(2) 0.0205(17) 0.0044(18) C12 0.095(3) 0.076(3) 0.0431(18) -0.0087(18) -0.0016(19) 0.007(2) C13 0.0554(19) 0.072(2) 0.062(2) 0.0310(19) 0.0130(16) 0.0213(17) C14 0.0423(14) 0.0323(13) 0.0469(14) -0.0030(11) 0.0150(12) -0.0088(11) C15 0.077(3) 0.056(2) 0.083(3) -0.0225(19) 0.039(2) -0.0034(18) C16 0.0462(17) 0.061(2) 0.072(2) -0.0063(19) 0.0041(16) -0.0166(16) C17 0.066(2) 0.054(2) 0.074(2) 0.0160(18) 0.0231(19) -0.0147(17) C18 0.0315(12) 0.0625(19) 0.0440(14) -0.0026(14) 0.0144(11) 0.0063(13) C19 0.0406(18) 0.148(5) 0.068(2) 0.004(3) 0.0095(17) 0.021(2) C20 0.076(3) 0.211(7) 0.119(4) 0.087(5) 0.062(3) 0.030(4) C21 0.088(4) 0.135(6) 0.264(10) -0.135(7) 0.042(5) 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 Nb1 O4 1.8616(18) . ? Nb1 O2 1.8797(18) . ? Nb1 O3 1.8841(18) . ? Nb1 O1 1.8892(18) . ? Nb1 N1 2.363(2) . ? Nb1 Cl1 2.5463(6) . ? O1 C14 1.412(3) . ? O2 C18 1.402(3) . ? N1 C1 1.339(3) . ? N1 C5 1.342(3) . ? O3 C6 1.424(3) . ? O4 C10 1.425(3) . ? C1 C2 1.385(4) . ? C2 C3 1.388(4) . ? C3 C4 1.377(4) . ? C4 C5 1.382(4) . ? C6 C9 1.515(4) . ? C6 C7 1.525(4) . ? C6 C8 1.530(4) . ? C10 C11 1.508(5) . ? C10 C13 1.518(4) . ? C10 C12 1.524(5) . ? C14 C17 1.515(5) . ? C14 C16 1.518(4) . ? C14 C15 1.522(5) . ? C18 C19 1.475(5) . ? C18 C21 1.485(6) . ? C18 C20 1.513(6) . ? 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 Nb1 O2 99.37(8) . . ? O4 Nb1 O3 97.50(8) . . ? O2 Nb1 O3 93.71(9) . . ? O4 Nb1 O1 97.88(9) . . ? O2 Nb1 O1 92.86(9) . . ? O3 Nb1 O1 162.04(8) . . ? O4 Nb1 N1 173.63(7) . . ? O2 Nb1 N1 86.91(8) . . ? O3 Nb1 N1 80.92(8) . . ? O1 Nb1 N1 82.77(8) . . ? O4 Nb1 Cl1 89.55(6) . . ? O2 Nb1 Cl1 171.06(6) . . ? O3 Nb1 Cl1 85.69(6) . . ? O1 Nb1 Cl1 85.23(6) . . ? N1 Nb1 Cl1 84.19(5) . . ? C14 O1 Nb1 171.35(18) . . ? C18 O2 Nb1 159.25(19) . . ? C1 N1 C5 117.6(2) . . ? C1 N1 Nb1 124.53(16) . . ? C5 N1 Nb1 117.88(17) . . ? C6 O3 Nb1 162.06(17) . . ? C10 O4 Nb1 160.48(18) . . ? N1 C1 C2 123.2(2) . . ? C1 C2 C3 118.4(3) . . ? C4 C3 C2 118.8(3) . . ? C3 C4 C5 119.2(3) . . ? N1 C5 C4 122.8(3) . . ? O3 C6 C9 107.9(2) . . ? O3 C6 C7 107.1(2) . . ? C9 C6 C7 110.2(3) . . ? O3 C6 C8 109.7(2) . . ? C9 C6 C8 111.1(3) . . ? C7 C6 C8 110.8(3) . . ? O4 C10 C11 107.9(2) . . ? O4 C10 C13 107.1(2) . . ? C11 C10 C13 111.3(3) . . ? O4 C10 C12 107.7(3) . . ? C11 C10 C12 110.9(3) . . ? C13 C10 C12 111.8(3) . . ? O1 C14 C17 108.9(3) . . ? O1 C14 C16 107.9(3) . . ? C17 C14 C16 110.2(3) . . ? O1 C14 C15 107.6(2) . . ? C17 C14 C15 111.4(3) . . ? C16 C14 C15 110.8(3) . . ? O2 C18 C19 109.6(3) . . ? O2 C18 C21 107.3(3) . . ? C19 C18 C21 112.5(5) . . ? O2 C18 C20 107.5(3) . . ? C19 C18 C20 109.6(4) . . ? C21 C18 C20 110.3(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.61 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.895 _refine_diff_density_min -1.107 _refine_diff_density_rms 0.118 # Attachment 'ap003.cif' data_003 _database_code_depnum_ccdc_archive 'CCDC 809951' #TrackingRef 'ap003.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H33 F3 N Nb O5' _chemical_formula_sum 'C20 H33 F3 N Nb O5' _chemical_formula_weight 517.38 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' F F 0.0171 0.0103 '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' Nb Nb -2.0727 0.6215 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 8.2345(10) _cell_length_b 18.8002(18) _cell_length_c 17.923(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.248(9) _cell_angle_gamma 90.00 _cell_volume 2488.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 22848 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 54.04 _exptl_crystal_description cylinder _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_size_rad 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.533 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(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 'IPDS II (Stoe & Cie)' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 10813 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0844 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.34 _reflns_number_total 5551 _reflns_number_gt 3211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _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^)+(0.0904P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0073(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5551 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1512 _refine_ls_wR_factor_gt 0.1407 _refine_ls_goodness_of_fit_ref 0.864 _refine_ls_restrained_S_all 0.864 _refine_ls_shift/su_max 0.000 _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 Nb1 Nb 0.61659(6) 0.12088(2) 0.26271(3) 0.04369(16) Uani 1 1 d . . . F1 F 1.0310(6) 0.29615(19) 0.3941(2) 0.1026(14) Uani 1 1 d . . . F2 F 1.0919(6) 0.2298(2) 0.4989(2) 0.1041(15) Uani 1 1 d . . . F3 F 1.2788(7) 0.2399(3) 0.4467(3) 0.1346(19) Uani 1 1 d . . . O1 O 0.4483(5) 0.06223(17) 0.1775(2) 0.0529(8) Uani 1 1 d . . . O2 O 0.6665(5) 0.17483(17) 0.1867(2) 0.0529(8) Uani 1 1 d . . . O3 O 0.4615(5) 0.18870(18) 0.2740(2) 0.0562(8) Uani 1 1 d . . . O4 O 0.8423(5) 0.16808(18) 0.3564(2) 0.0595(9) Uani 1 1 d . . . O5 O 0.6265(4) 0.05708(17) 0.3461(2) 0.0495(8) Uani 1 1 d . . . N1 N 0.8564(6) 0.0489(2) 0.2638(2) 0.0485(9) Uani 1 1 d . . . C1 C 0.8032(8) -0.0136(3) 0.2241(3) 0.0583(13) Uani 1 1 d . . . H1 H 0.6834 -0.0274 0.2063 0.070 Uiso 1 1 calc R . . C2 C 0.9174(10) -0.0584(3) 0.2082(4) 0.0730(17) Uani 1 1 d . . . H2 H 0.8751 -0.1013 0.1805 0.088 Uiso 1 1 calc R . . C3 C 1.0945(10) -0.0382(3) 0.2342(4) 0.0787(19) Uani 1 1 d . . . H3 H 1.1735 -0.0667 0.2230 0.094 Uiso 1 1 calc R . . C4 C 1.1525(8) 0.0237(3) 0.2763(4) 0.0704(17) Uani 1 1 d . . . H4 H 1.2724 0.0376 0.2945 0.084 Uiso 1 1 calc R . . C5 C 1.0329(7) 0.0675(3) 0.2928(3) 0.0548(12) Uani 1 1 d . . . C6 C 1.1020(7) 0.1308(3) 0.3427(3) 0.0617(14) Uani 1 1 d . . . H6 H 1.2216 0.1430 0.3570 0.074 Uiso 1 1 calc R . . C7 C 1.0102(8) 0.1736(3) 0.3703(3) 0.0566(13) Uani 1 1 d . . . C8 C 1.1044(10) 0.2340(4) 0.4275(4) 0.0791(19) Uani 1 1 d . . . C9 C 0.7763(8) 0.2055(3) 0.1515(3) 0.0534(12) Uani 1 1 d . . . H9 H 0.9035 0.1939 0.1871 0.064 Uiso 1 1 calc R . . C10 C 0.7231(10) 0.1751(5) 0.0677(4) 0.094(2) Uani 1 1 d . . . H10A H 0.7403 0.1244 0.0721 0.142 Uiso 1 1 calc R . . H10B H 0.7966 0.1955 0.0440 0.142 Uiso 1 1 calc R . . H10C H 0.5981 0.1855 0.0327 0.142 Uiso 1 1 calc R . . C11 C 0.7526(12) 0.2859(3) 0.1492(6) 0.101(3) Uani 1 1 d . . . H11A H 0.7884 0.3033 0.2046 0.151 Uiso 1 1 calc R . . H11B H 0.6279 0.2976 0.1150 0.151 Uiso 1 1 calc R . . H11C H 0.8266 0.3074 0.1264 0.151 Uiso 1 1 calc R . . C12 C 0.4267(10) 0.2638(3) 0.2502(5) 0.082(2) Uani 1 1 d . . . H12 H 0.4685 0.2732 0.2078 0.099 Uiso 1 1 calc R . . C13 C 0.5363(12) 0.3080(4) 0.3241(6) 0.121(3) Uani 1 1 d . . . H13A H 0.6621 0.2963 0.3440 0.181 Uiso 1 1 calc R . . H13B H 0.4995 0.2989 0.3671 0.181 Uiso 1 1 calc R . . H13C H 0.5182 0.3574 0.3091 0.181 Uiso 1 1 calc R . . C14 C 0.2311(10) 0.2777(4) 0.2132(5) 0.090(2) Uani 1 1 d . . . H14A H 0.1703 0.2472 0.1659 0.134 Uiso 1 1 calc R . . H14B H 0.2084 0.3265 0.1959 0.134 Uiso 1 1 calc R . . H14C H 0.1869 0.2684 0.2536 0.134 Uiso 1 1 calc R . . C15 C 0.3395(9) 0.0678(3) 0.0895(3) 0.0710(17) Uani 1 1 d . . . H15 H 0.3930 0.1032 0.0668 0.085 Uiso 1 1 calc R . . C16 C 0.1513(12) 0.0925(4) 0.0746(5) 0.114(3) Uani 1 1 d . . . H16A H 0.1601 0.1378 0.1009 0.172 Uiso 1 1 calc R . . H16B H 0.0993 0.0583 0.0976 0.172 Uiso 1 1 calc R . . H16C H 0.0758 0.0969 0.0159 0.172 Uiso 1 1 calc R . . C17 C 0.3303(13) -0.0004(6) 0.0495(5) 0.145(4) Uani 1 1 d . . . H17A H 0.4500 -0.0150 0.0596 0.217 Uiso 1 1 calc R . . H17B H 0.2562 0.0040 -0.0093 0.217 Uiso 1 1 calc R . . H17C H 0.2786 -0.0353 0.0718 0.217 Uiso 1 1 calc R . . C18 C 0.7414(8) 0.0252(3) 0.4233(3) 0.0622(14) Uani 1 1 d . . . H18 H 0.8660 0.0264 0.4298 0.075 Uiso 1 1 calc R . . C19 C 0.6866(12) -0.0509(4) 0.4230(5) 0.103(3) Uani 1 1 d . . . H19A H 0.6942 -0.0756 0.3778 0.154 Uiso 1 1 calc R . . H19B H 0.5644 -0.0528 0.4163 0.154 Uiso 1 1 calc R . . H19C H 0.7660 -0.0730 0.4746 0.154 Uiso 1 1 calc R . . C20 C 0.7334(14) 0.0666(4) 0.4922(4) 0.111(3) Uani 1 1 d . . . H20A H 0.7679 0.1150 0.4895 0.166 Uiso 1 1 calc R . . H20B H 0.8150 0.0462 0.5445 0.166 Uiso 1 1 calc R . . H20C H 0.6123 0.0655 0.4870 0.166 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 Nb1 0.0481(3) 0.0406(2) 0.0445(2) 0.00144(19) 0.02233(17) -0.0012(2) F1 0.138(4) 0.061(2) 0.080(2) 0.0002(18) 0.022(2) -0.032(2) F2 0.151(4) 0.092(3) 0.0498(19) -0.0109(18) 0.027(2) -0.041(3) F3 0.091(3) 0.152(4) 0.133(4) -0.043(3) 0.024(3) -0.058(3) O1 0.058(2) 0.0489(18) 0.0512(18) 0.0022(15) 0.0241(16) -0.0043(16) O2 0.066(2) 0.0420(16) 0.0526(18) 0.0069(14) 0.0283(17) 0.0023(16) O3 0.051(2) 0.0550(19) 0.066(2) -0.0021(17) 0.0295(17) 0.0040(17) O4 0.066(2) 0.056(2) 0.057(2) -0.0054(16) 0.0276(18) -0.0123(18) O5 0.0426(18) 0.0552(19) 0.0543(19) 0.0024(15) 0.0248(15) -0.0016(15) N1 0.055(3) 0.043(2) 0.051(2) 0.0114(17) 0.0276(19) 0.0050(18) C1 0.069(3) 0.044(3) 0.070(3) 0.001(2) 0.039(3) 0.002(2) C2 0.098(5) 0.048(3) 0.094(4) 0.007(3) 0.062(4) 0.013(3) C3 0.091(5) 0.068(4) 0.105(5) 0.030(3) 0.068(4) 0.029(4) C4 0.063(4) 0.071(4) 0.093(4) 0.028(3) 0.049(4) 0.011(3) C5 0.052(3) 0.056(3) 0.061(3) 0.022(2) 0.030(2) 0.005(2) C6 0.043(3) 0.072(4) 0.061(3) 0.014(3) 0.015(2) -0.011(3) C7 0.054(3) 0.066(3) 0.042(3) 0.010(2) 0.015(2) -0.011(3) C8 0.084(5) 0.083(4) 0.054(3) 0.002(3) 0.015(3) -0.026(4) C9 0.062(3) 0.055(3) 0.045(3) 0.012(2) 0.025(2) 0.002(2) C10 0.090(5) 0.142(7) 0.068(4) -0.020(4) 0.050(4) -0.011(5) C11 0.131(7) 0.056(4) 0.151(7) 0.024(4) 0.094(6) 0.000(4) C12 0.086(5) 0.053(3) 0.114(5) -0.013(3) 0.050(4) 0.010(3) C13 0.107(6) 0.076(5) 0.143(7) -0.049(5) 0.022(6) 0.003(4) C14 0.092(5) 0.063(4) 0.104(5) 0.005(4) 0.034(4) 0.016(4) C15 0.074(4) 0.079(4) 0.046(3) 0.003(3) 0.014(3) -0.029(3) C16 0.119(7) 0.105(6) 0.071(5) 0.000(4) -0.002(4) 0.035(5) C17 0.115(7) 0.187(10) 0.078(5) -0.062(6) -0.007(5) 0.052(7) C18 0.068(4) 0.071(3) 0.049(3) 0.018(2) 0.027(3) 0.010(3) C19 0.141(7) 0.076(5) 0.080(5) 0.028(4) 0.039(5) 0.009(4) C20 0.175(9) 0.108(6) 0.058(4) 0.003(4) 0.060(5) 0.006(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O3 1.878(3) . ? Nb1 O2 1.883(3) . ? Nb1 O5 1.889(3) . ? Nb1 O1 1.897(3) . ? Nb1 O4 2.074(4) . ? Nb1 N1 2.387(4) . ? F1 C8 1.330(8) . ? F2 C8 1.330(7) . ? F3 C8 1.325(8) . ? O1 C15 1.433(6) . ? O2 C9 1.433(6) . ? O3 C12 1.466(7) . ? O4 C7 1.297(6) . ? O5 C18 1.419(6) . ? N1 C1 1.343(6) . ? N1 C5 1.355(6) . ? C1 C2 1.382(8) . ? C1 H1 0.9300 . ? C2 C3 1.373(9) . ? C2 H2 0.9300 . ? C3 C4 1.355(9) . ? C3 H3 0.9300 . ? C4 C5 1.411(8) . ? C4 H4 0.9300 . ? C5 C6 1.446(8) . ? C6 C7 1.339(8) . ? C6 H6 0.9300 . ? C7 C8 1.496(8) . ? C9 C10 1.481(8) . ? C9 C11 1.522(8) . ? C9 H9 0.9800 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C14 1.469(9) . ? C12 C13 1.484(9) . ? C12 H12 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C17 1.455(10) . ? C15 C16 1.524(11) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C20 1.485(9) . ? C18 C19 1.500(9) . ? C18 H18 0.9800 . ? 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 O3 Nb1 O2 95.06(15) . . ? O3 Nb1 O5 98.03(15) . . ? O2 Nb1 O5 165.18(14) . . ? O3 Nb1 O1 101.07(16) . . ? O2 Nb1 O1 92.65(14) . . ? O5 Nb1 O1 91.62(14) . . ? O3 Nb1 O4 91.77(15) . . ? O2 Nb1 O4 87.20(14) . . ? O5 Nb1 O4 85.50(14) . . ? O1 Nb1 O4 167.12(15) . . ? O3 Nb1 N1 169.64(15) . . ? O2 Nb1 N1 82.34(14) . . ? O5 Nb1 N1 83.55(13) . . ? O1 Nb1 N1 89.09(15) . . ? O4 Nb1 N1 78.12(15) . . ? C15 O1 Nb1 136.3(3) . . ? C9 O2 Nb1 156.5(3) . . ? C12 O3 Nb1 132.7(4) . . ? C7 O4 Nb1 133.4(3) . . ? C18 O5 Nb1 144.8(3) . . ? C1 N1 C5 118.1(5) . . ? C1 N1 Nb1 114.6(4) . . ? C5 N1 Nb1 126.9(3) . . ? N1 C1 C2 123.4(6) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 118.6(6) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C4 C3 C2 119.1(6) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 120.7(6) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? N1 C5 C4 120.0(5) . . ? N1 C5 C6 120.7(5) . . ? C4 C5 C6 119.3(5) . . ? C7 C6 C5 126.3(5) . . ? C7 C6 H6 116.9 . . ? C5 C6 H6 116.9 . . ? O4 C7 C6 127.5(5) . . ? O4 C7 C8 112.2(6) . . ? C6 C7 C8 120.2(6) . . ? F3 C8 F2 107.0(5) . . ? F3 C8 F1 105.5(6) . . ? F2 C8 F1 105.8(6) . . ? F3 C8 C7 114.5(6) . . ? F2 C8 C7 112.2(5) . . ? F1 C8 C7 111.3(5) . . ? O2 C9 C10 109.3(5) . . ? O2 C9 C11 108.3(5) . . ? C10 C9 C11 112.3(6) . . ? O2 C9 H9 109.0 . . ? C10 C9 H9 109.0 . . ? C11 C9 H9 109.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O3 C12 C14 109.6(6) . . ? O3 C12 C13 108.4(6) . . ? C14 C12 C13 114.6(6) . . ? O3 C12 H12 108.0 . . ? C14 C12 H12 108.0 . . ? C13 C12 H12 108.0 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 C15 C17 110.4(6) . . ? O1 C15 C16 107.9(5) . . ? C17 C15 C16 110.8(6) . . ? O1 C15 H15 109.2 . . ? C17 C15 H15 109.2 . . ? C16 C15 H15 109.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O5 C18 C20 109.5(5) . . ? O5 C18 C19 109.2(5) . . ? C20 C18 C19 112.3(6) . . ? O5 C18 H18 108.6 . . ? C20 C18 H18 108.6 . . ? C19 C18 H18 108.6 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 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 O3 Nb1 O1 C15 73.4(5) . . . . ? O2 Nb1 O1 C15 -22.3(5) . . . . ? O5 Nb1 O1 C15 171.9(5) . . . . ? O4 Nb1 O1 C15 -111.4(7) . . . . ? N1 Nb1 O1 C15 -104.6(5) . . . . ? O3 Nb1 O2 C9 135.9(7) . . . . ? O5 Nb1 O2 C9 -16.1(11) . . . . ? O1 Nb1 O2 C9 -122.7(8) . . . . ? O4 Nb1 O2 C9 44.4(7) . . . . ? N1 Nb1 O2 C9 -34.0(7) . . . . ? O2 Nb1 O3 C12 -13.8(5) . . . . ? O5 Nb1 O3 C12 159.3(5) . . . . ? O1 Nb1 O3 C12 -107.5(5) . . . . ? O4 Nb1 O3 C12 73.6(5) . . . . ? N1 Nb1 O3 C12 61.1(10) . . . . ? O3 Nb1 O4 C7 -148.9(5) . . . . ? O2 Nb1 O4 C7 -53.9(4) . . . . ? O5 Nb1 O4 C7 113.2(5) . . . . ? O1 Nb1 O4 C7 35.7(9) . . . . ? N1 Nb1 O4 C7 28.8(4) . . . . ? O3 Nb1 O5 C18 -117.0(6) . . . . ? O2 Nb1 O5 C18 34.9(9) . . . . ? O1 Nb1 O5 C18 141.6(6) . . . . ? O4 Nb1 O5 C18 -25.8(6) . . . . ? N1 Nb1 O5 C18 52.7(6) . . . . ? O3 Nb1 N1 C1 176.6(7) . . . . ? O2 Nb1 N1 C1 -107.3(3) . . . . ? O5 Nb1 N1 C1 77.2(3) . . . . ? O1 Nb1 N1 C1 -14.5(3) . . . . ? O4 Nb1 N1 C1 163.9(3) . . . . ? O3 Nb1 N1 C5 -9.9(10) . . . . ? O2 Nb1 N1 C5 66.1(4) . . . . ? O5 Nb1 N1 C5 -109.3(4) . . . . ? O1 Nb1 N1 C5 158.9(4) . . . . ? O4 Nb1 N1 C5 -22.6(4) . . . . ? C5 N1 C1 C2 -3.0(7) . . . . ? Nb1 N1 C1 C2 171.1(4) . . . . ? N1 C1 C2 C3 0.0(9) . . . . ? C1 C2 C3 C4 1.7(9) . . . . ? C2 C3 C4 C5 -0.5(9) . . . . ? C1 N1 C5 C4 4.1(7) . . . . ? Nb1 N1 C5 C4 -169.1(3) . . . . ? C1 N1 C5 C6 -174.2(4) . . . . ? Nb1 N1 C5 C6 12.5(6) . . . . ? C3 C4 C5 N1 -2.5(8) . . . . ? C3 C4 C5 C6 175.9(5) . . . . ? N1 C5 C6 C7 5.2(8) . . . . ? C4 C5 C6 C7 -173.2(5) . . . . ? Nb1 O4 C7 C6 -24.4(8) . . . . ? Nb1 O4 C7 C8 158.9(4) . . . . ? C5 C6 C7 O4 -1.7(9) . . . . ? C5 C6 C7 C8 174.7(5) . . . . ? O4 C7 C8 F3 177.0(5) . . . . ? C6 C7 C8 F3 0.1(8) . . . . ? O4 C7 C8 F2 54.9(7) . . . . ? C6 C7 C8 F2 -122.1(6) . . . . ? O4 C7 C8 F1 -63.4(7) . . . . ? C6 C7 C8 F1 119.6(6) . . . . ? Nb1 O2 C9 C10 115.3(8) . . . . ? Nb1 O2 C9 C11 -122.1(8) . . . . ? Nb1 O3 C12 C14 137.0(5) . . . . ? Nb1 O3 C12 C13 -97.2(7) . . . . ? Nb1 O1 C15 C17 143.1(6) . . . . ? Nb1 O1 C15 C16 -95.8(6) . . . . ? Nb1 O5 C18 C20 95.2(7) . . . . ? Nb1 O5 C18 C19 -141.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.34 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.271 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.125 data_la005 _database_code_depnum_ccdc_archive 'CCDC 853078' #TrackingRef 'la005.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H33 F3 N Nb O5 S' _chemical_formula_sum 'C22 H33 F3 N Nb O5 S' _chemical_formula_weight 573.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 10.2154(9) _cell_length_b 15.3306(16) _cell_length_c 17.1146(14) _cell_angle_alpha 90.00 _cell_angle_beta 95.429(7) _cell_angle_gamma 90.00 _cell_volume 2668.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 20191 _cell_measurement_theta_min 3.41 _cell_measurement_theta_max 54.17 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.580 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5386 _exptl_absorpt_correction_T_max 0.8662 _exptl_absorpt_process_details ; The absorption correction (X-RED; Stoe & Cie, 2001) was performed after optimizing the crytal shape using X-SHAPE (Soe & Cie, 1999). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(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 'IPDS II (Stoe & Cie)' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 32478 _diffrn_reflns_av_R_equivalents 0.1181 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.37 _reflns_number_total 5950 _reflns_number_gt 4204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _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^)+(0.0702P)^2^+1.7628P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0069(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5950 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1264 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _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 Nb1 Nb 0.15171(3) 0.269022(18) 0.690344(18) 0.03476(12) Uani 1 1 d . . . S1 S 0.19744(10) 0.00886(6) 0.85365(6) 0.0473(2) Uani 1 1 d . . . F3 F 0.3420(2) -0.03227(13) 0.57484(15) 0.0575(6) Uani 1 1 d . . . F2 F 0.2956(3) 0.08384(16) 0.50799(14) 0.0631(6) Uani 1 1 d . . . O2 O 0.1519(2) 0.33035(15) 0.59544(14) 0.0418(6) Uani 1 1 d . . . F1 F 0.4783(2) 0.07464(17) 0.58092(16) 0.0641(6) Uani 1 1 d . . . O5 O 0.3062(2) 0.31521(14) 0.74593(14) 0.0395(5) Uani 1 1 d . . . O3 O 0.0098(2) 0.19537(15) 0.65718(14) 0.0410(5) Uani 1 1 d . . . O4 O 0.0439(2) 0.34609(15) 0.74275(15) 0.0428(6) Uani 1 1 d . . . O1 O 0.2738(2) 0.17833(14) 0.63837(15) 0.0414(5) Uani 1 1 d . . . N1 N 0.1809(3) 0.16186(17) 0.78853(17) 0.0361(6) Uani 1 1 d . . . C5 C 0.1542(4) 0.0958(2) 0.9103(2) 0.0426(8) Uani 1 1 d . . . C3 C 0.2565(3) 0.0440(2) 0.7050(2) 0.0392(7) Uani 1 1 d . . . H3 H 0.2662 -0.0161 0.7011 0.047 Uiso 1 1 calc R . . C10 C 0.1523(3) 0.1732(2) 0.8665(2) 0.0388(7) Uani 1 1 d . . . C4 C 0.2105(3) 0.0793(2) 0.7749(2) 0.0392(7) Uani 1 1 d . . . C17 C -0.0890(4) 0.3749(2) 0.7327(2) 0.0498(9) Uani 1 1 d . . . H17 H -0.1407 0.3327 0.6996 0.060 Uiso 1 1 calc R . . C2 C 0.2863(3) 0.0943(2) 0.6451(2) 0.0369(7) Uani 1 1 d . . . C1 C 0.3499(4) 0.0545(2) 0.5773(2) 0.0460(8) Uani 1 1 d . . . C8 C 0.1025(5) 0.2514(3) 0.9806(3) 0.0561(10) Uani 1 1 d . . . H8 H 0.0865 0.3037 1.0054 0.067 Uiso 1 1 calc R . . C9 C 0.1268(4) 0.2522(2) 0.9022(2) 0.0457(9) Uani 1 1 d . . . H020 H 0.1260 0.3042 0.8741 0.055 Uiso 1 1 calc R . . C14 C -0.0678(4) 0.1186(2) 0.6544(2) 0.0456(8) Uani 1 1 d . . . H14 H -0.0210 0.0743 0.6876 0.055 Uiso 1 1 calc R . . C6 C 0.1278(4) 0.0955(3) 0.9887(2) 0.0556(10) Uani 1 1 d . . . H6 H 0.1280 0.0438 1.0172 0.067 Uiso 1 1 calc R . . C20 C 0.4262(4) 0.2922(3) 0.7889(2) 0.0498(9) Uani 1 1 d . . . H20 H 0.4115 0.2362 0.8144 0.060 Uiso 1 1 calc R . . C11 C 0.1175(4) 0.3110(3) 0.5142(2) 0.0480(9) Uani 1 1 d . . . H11 H 0.1051 0.2478 0.5088 0.058 Uiso 1 1 calc R . . C21 C 0.4611(4) 0.3559(3) 0.8523(3) 0.0569(10) Uani 1 1 d . . . H21A H 0.3910 0.3595 0.8858 0.085 Uiso 1 1 calc R . . H21B H 0.4748 0.4122 0.8298 0.085 Uiso 1 1 calc R . . H21C H 0.5402 0.3375 0.8825 0.085 Uiso 1 1 calc R . . C7 C 0.1016(5) 0.1740(3) 1.0227(3) 0.0615(11) Uani 1 1 d . . . H7 H 0.0830 0.1754 1.0748 0.074 Uiso 1 1 calc R . . C19 C -0.1435(4) 0.3791(3) 0.8118(3) 0.0621(11) Uani 1 1 d . . . H19A H -0.1383 0.3224 0.8358 0.093 Uiso 1 1 calc R . . H19B H -0.2336 0.3976 0.8050 0.093 Uiso 1 1 calc R . . H19C H -0.0931 0.4199 0.8449 0.093 Uiso 1 1 calc R . . C18 C -0.0931(5) 0.4626(3) 0.6908(3) 0.0671(12) Uani 1 1 d . . . H18A H -0.0582 0.4562 0.6409 0.101 Uiso 1 1 calc R . . H18B H -0.0412 0.5041 0.7222 0.101 Uiso 1 1 calc R . . H18C H -0.1823 0.4827 0.6828 0.101 Uiso 1 1 calc R . . C15 C -0.0850(6) 0.0851(3) 0.5724(3) 0.0760(14) Uani 1 1 d . . . H15A H -0.0005 0.0728 0.5548 0.114 Uiso 1 1 calc R . . H15B H -0.1293 0.1282 0.5389 0.114 Uiso 1 1 calc R . . H15C H -0.1365 0.0326 0.5707 0.114 Uiso 1 1 calc R . . C22 C 0.5282(5) 0.2777(5) 0.7370(4) 0.117(3) Uani 1 1 d . . . H22A H 0.4988 0.2351 0.6981 0.176 Uiso 1 1 calc R . . H22B H 0.6063 0.2570 0.7668 0.176 Uiso 1 1 calc R . . H22C H 0.5471 0.3315 0.7116 0.176 Uiso 1 1 calc R . . C16 C -0.1954(5) 0.1373(3) 0.6864(4) 0.0860(17) Uani 1 1 d . . . H16A H -0.1792 0.1588 0.7390 0.129 Uiso 1 1 calc R . . H16B H -0.2464 0.0847 0.6864 0.129 Uiso 1 1 calc R . . H16C H -0.2427 0.1803 0.6542 0.129 Uiso 1 1 calc R . . C13 C -0.0106(6) 0.3548(4) 0.4886(3) 0.096(2) Uani 1 1 d . . . H13A H -0.0772 0.3341 0.5200 0.144 Uiso 1 1 calc R . . H13B H -0.0356 0.3416 0.4344 0.144 Uiso 1 1 calc R . . H13C H -0.0010 0.4168 0.4949 0.144 Uiso 1 1 calc R . . C12 C 0.2261(7) 0.3368(5) 0.4686(3) 0.108(2) Uani 1 1 d . . . H12A H 0.3045 0.3061 0.4878 0.162 Uiso 1 1 calc R . . H12B H 0.2407 0.3985 0.4739 0.162 Uiso 1 1 calc R . . H12C H 0.2040 0.3228 0.4143 0.162 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 Nb1 0.03791(17) 0.02586(16) 0.03924(19) -0.00045(12) -0.00292(11) -0.00001(11) S1 0.0626(6) 0.0321(4) 0.0472(6) 0.0057(4) 0.0048(4) 0.0040(4) F3 0.0749(16) 0.0343(11) 0.0665(16) -0.0076(10) 0.0224(12) 0.0038(10) F2 0.0888(18) 0.0557(14) 0.0443(13) -0.0018(11) 0.0043(12) 0.0132(13) O2 0.0495(14) 0.0318(11) 0.0422(14) -0.0004(10) -0.0052(11) -0.0020(10) F1 0.0521(14) 0.0626(14) 0.0810(18) -0.0079(13) 0.0244(12) -0.0053(11) O5 0.0398(12) 0.0307(11) 0.0464(14) -0.0015(10) -0.0047(10) -0.0007(9) O3 0.0436(13) 0.0336(12) 0.0448(14) 0.0001(10) -0.0009(10) -0.0017(10) O4 0.0438(13) 0.0353(12) 0.0479(15) -0.0013(10) -0.0024(11) 0.0027(10) O1 0.0481(14) 0.0282(11) 0.0486(15) 0.0006(10) 0.0072(11) 0.0010(10) N1 0.0398(14) 0.0281(13) 0.0398(16) 0.0007(11) 0.0010(11) 0.0010(11) C5 0.047(2) 0.0410(18) 0.0393(19) 0.0031(14) 0.0022(15) 0.0013(15) C3 0.0428(18) 0.0269(15) 0.048(2) -0.0013(14) 0.0030(15) 0.0027(13) C10 0.0412(18) 0.0353(16) 0.0392(19) -0.0014(14) 0.0000(14) -0.0009(13) C4 0.0419(18) 0.0329(16) 0.0424(19) -0.0014(14) 0.0015(14) -0.0008(14) C17 0.0419(19) 0.0423(19) 0.063(3) -0.0117(18) -0.0063(17) 0.0094(15) C2 0.0354(16) 0.0309(15) 0.0439(19) -0.0048(13) 0.0014(14) 0.0006(12) C1 0.050(2) 0.0339(17) 0.055(2) -0.0001(15) 0.0083(17) 0.0009(15) C8 0.067(3) 0.052(2) 0.049(2) -0.0106(18) 0.0072(19) 0.0065(19) C9 0.052(2) 0.0372(18) 0.048(2) -0.0017(15) 0.0024(17) 0.0035(15) C14 0.0419(19) 0.0353(17) 0.059(2) -0.0005(16) -0.0005(16) -0.0069(14) C6 0.069(3) 0.051(2) 0.048(2) 0.0087(18) 0.0104(19) 0.0006(19) C20 0.0399(19) 0.053(2) 0.054(2) -0.0037(18) -0.0058(16) 0.0039(16) C11 0.059(2) 0.043(2) 0.040(2) -0.0027(16) -0.0043(17) 0.0029(17) C21 0.047(2) 0.068(3) 0.052(2) -0.013(2) -0.0090(18) 0.0091(19) C7 0.080(3) 0.061(3) 0.045(2) -0.0006(19) 0.010(2) 0.004(2) C19 0.047(2) 0.064(3) 0.076(3) -0.003(2) 0.011(2) 0.0009(19) C18 0.067(3) 0.060(3) 0.074(3) 0.006(2) 0.007(2) 0.029(2) C15 0.089(4) 0.059(3) 0.076(3) -0.013(2) -0.015(3) -0.016(3) C22 0.042(3) 0.211(8) 0.097(5) -0.092(5) 0.003(3) 0.002(4) C16 0.063(3) 0.063(3) 0.137(5) 0.001(3) 0.034(3) -0.012(2) C13 0.097(4) 0.120(5) 0.062(3) -0.022(3) -0.035(3) 0.044(4) C12 0.101(5) 0.167(7) 0.061(4) -0.013(4) 0.029(3) -0.042(5) _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 Nb1 O2 1.877(2) . ? Nb1 O3 1.882(2) . ? Nb1 O4 1.898(2) . ? Nb1 O5 1.901(2) . ? Nb1 O1 2.119(2) . ? Nb1 N1 2.349(3) . ? S1 C5 1.730(4) . ? S1 C4 1.742(4) . ? F3 C1 1.333(4) . ? F2 C1 1.338(4) . ? O2 C11 1.432(4) . ? F1 C1 1.343(4) . ? O5 C20 1.413(4) . ? O3 C14 1.418(4) . ? O4 C17 1.422(4) . ? O1 C2 1.298(4) . ? N1 C4 1.327(4) . ? N1 C10 1.404(5) . ? C5 C6 1.394(6) . ? C5 C10 1.403(5) . ? C3 C2 1.342(5) . ? C3 C4 1.432(5) . ? C10 C9 1.392(5) . ? C17 C19 1.514(6) . ? C17 C18 1.523(6) . ? C2 C1 1.512(5) . ? C8 C9 1.388(6) . ? C8 C7 1.388(6) . ? C14 C15 1.488(6) . ? C14 C16 1.488(6) . ? C6 C7 1.374(6) . ? C20 C22 1.450(6) . ? C20 C21 1.478(5) . ? C11 C12 1.470(7) . ? C11 C13 1.499(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nb1 O3 95.95(10) . . ? O2 Nb1 O4 98.37(11) . . ? O3 Nb1 O4 92.92(10) . . ? O2 Nb1 O5 100.22(10) . . ? O3 Nb1 O5 162.49(10) . . ? O4 Nb1 O5 91.33(10) . . ? O2 Nb1 O1 85.20(10) . . ? O3 Nb1 O1 86.96(10) . . ? O4 Nb1 O1 176.42(10) . . ? O5 Nb1 O1 87.75(10) . . ? O2 Nb1 N1 163.54(10) . . ? O3 Nb1 N1 80.69(10) . . ? O4 Nb1 N1 97.90(10) . . ? O5 Nb1 N1 81.91(10) . . ? O1 Nb1 N1 78.55(10) . . ? C5 S1 C4 89.92(17) . . ? C11 O2 Nb1 135.7(2) . . ? C20 O5 Nb1 143.7(2) . . ? C14 O3 Nb1 157.0(2) . . ? C17 O4 Nb1 136.5(2) . . ? C2 O1 Nb1 132.1(2) . . ? C4 N1 C10 110.9(3) . . ? C4 N1 Nb1 123.8(2) . . ? C10 N1 Nb1 124.7(2) . . ? C6 C5 C10 121.6(3) . . ? C6 C5 S1 128.3(3) . . ? C10 C5 S1 110.1(3) . . ? C2 C3 C4 122.5(3) . . ? C9 C10 C5 119.7(3) . . ? C9 C10 N1 126.1(3) . . ? C5 C10 N1 114.2(3) . . ? N1 C4 C3 127.3(3) . . ? N1 C4 S1 114.8(3) . . ? C3 C4 S1 117.8(2) . . ? O4 C17 C19 109.4(3) . . ? O4 C17 C18 108.3(3) . . ? C19 C17 C18 112.8(4) . . ? O1 C2 C3 127.7(3) . . ? O1 C2 C1 112.2(3) . . ? C3 C2 C1 120.0(3) . . ? F3 C1 F2 106.8(3) . . ? F3 C1 F1 106.6(3) . . ? F2 C1 F1 106.6(3) . . ? F3 C1 C2 113.4(3) . . ? F2 C1 C2 111.9(3) . . ? F1 C1 C2 111.1(3) . . ? C9 C8 C7 121.4(4) . . ? C8 C9 C10 118.3(4) . . ? O3 C14 C15 109.6(3) . . ? O3 C14 C16 109.5(3) . . ? C15 C14 C16 112.5(4) . . ? C7 C6 C5 117.9(4) . . ? O5 C20 C22 110.9(4) . . ? O5 C20 C21 110.7(3) . . ? C22 C20 C21 114.4(4) . . ? O2 C11 C12 109.3(4) . . ? O2 C11 C13 108.6(3) . . ? C12 C11 C13 113.9(5) . . ? C6 C7 C8 121.1(4) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.37 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.687 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.097