Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Dr W. Edward Lindsell Department of Chemistry Heriot-Watt University Edinburgh EH14 4AS ; _publ_contact_author_phone '0131 451-8028' _publ_contact_author_fax '0131 451 3180' _publ_contact_author_email W.E.Lindsell@hw.ac.uk _publ_requested_journal 'Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_Cambridge 186 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? # 3. TITLE AND AUTHOR LIST _publ_section_title ;Synthesis and Structures of Monocyclopentadienylniobium complexes with Bi- and Tri-dentate Ligands ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Dersch, Roland K.' ; Department of Chemistry Heriot-Watt University Edinburgh EH14 4AS UK ; 'Jungclass, Henrik' ; Department of Chemistry Heriot-Watt University Edinburgh EH14 4AS UK ; 'Rosair, Georgina M.' ; Department of Chemistry Heriot-Watt University Edinburgh EH14 4AS UK ; 'Lindsell, W. Edward' ; Department of Chemistry Heriot-Watt University Edinburgh EH14 4AS UK ; #= data_1(194704) _database_code_CSD 194704 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety "(Nb 5+), (C5 H5 1-), (S4 C6 H12 2-)" _chemical_formula_sum 'C11 H17 Nb S4' _chemical_formula_weight 370.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Nb' 'Nb' -2.0727 0.6215 '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' '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' _symmetry_cell_setting Monoclinic _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 10.101(3) _cell_length_b 12.739(4) _cell_length_c 11.188(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.37(3) _cell_angle_gamma 90.00 _cell_volume 1433.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 12.88 _exptl_crystal_description plate _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 1.394 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.3844 _exptl_absorpt_correction_T_max 0.7330 _exptl_absorpt_process_details 'North et al., 1968' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3244 _diffrn_reflns_av_R_equivalents 0.1721 _diffrn_reflns_av_sigmaI/netI 0.1635 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2508 _reflns_number_gt 1353 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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 w1/[\s^2^(Fo^2^)+(0.2000P)^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 2508 _refine_ls_number_parameters 116 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2239 _refine_ls_R_factor_gt 0.1275 _refine_ls_wR_factor_ref 0.4358 _refine_ls_wR_factor_gt 0.3060 _refine_ls_goodness_of_fit_ref 1.389 _refine_ls_restrained_S_all 1.389 _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 0.22639(19) 0.75142(15) 0.48566(18) 0.0233(7) Uani 1 1 d . . . S2 S 0.2920(6) 0.8697(5) 0.6486(5) 0.0312(15) Uani 1 1 d . . . S1 S 0.1545(6) 0.9100(5) 0.3754(6) 0.0358(16) Uani 1 1 d . . . C1 C 0.288(3) 1.002(2) 0.410(2) 0.043(7) Uani 1 1 d . . . H1A H 0.3731 0.9638 0.4159 0.051 Uiso 1 1 calc R . . H1B H 0.2885 1.0525 0.3422 0.051 Uiso 1 1 calc R . . C2 C 0.277(3) 1.0653(18) 0.529(3) 0.052(8) Uani 1 1 d . . . H2A H 0.3670 1.0894 0.5603 0.062 Uiso 1 1 calc R . . H2B H 0.2209 1.1281 0.5114 0.062 Uiso 1 1 calc R . . C3 C 0.217(3) 0.9972(18) 0.623(2) 0.038(7) Uani 1 1 d . . . H3A H 0.1215 0.9875 0.5986 0.046 Uiso 1 1 calc R . . H3B H 0.2250 1.0359 0.7004 0.046 Uiso 1 1 calc R . . S3 S 0.3689(6) 0.7414(5) 0.3237(5) 0.0325(15) Uani 1 1 d . . . S4 S 0.3921(6) 0.6463(4) 0.5984(5) 0.0290(15) Uani 1 1 d . . . C4 C 0.483(3) 0.6300(19) 0.349(2) 0.042(7) Uani 1 1 d . . . H4A H 0.4337 0.5671 0.3715 0.051 Uiso 1 1 calc R . . H4B H 0.5245 0.6140 0.2740 0.051 Uiso 1 1 calc R . . C6 C 0.549(3) 0.707(2) 0.564(3) 0.049(7) Uiso 1 1 d . . . H6A H 0.5372 0.7835 0.5533 0.058 Uiso 1 1 calc R . . H6B H 0.6187 0.6948 0.6311 0.058 Uiso 1 1 calc R . . C5 C 0.591(3) 0.658(2) 0.449(3) 0.053(8) Uiso 1 1 d . . . H5A H 0.6412 0.5930 0.4718 0.064 Uiso 1 1 calc R . . H5B H 0.6540 0.7069 0.4155 0.064 Uiso 1 1 calc R . . C11 C -0.001(2) 0.7228(15) 0.5417(18) 0.037(6) Uani 1 1 d G . . H11 H -0.0404 0.7721 0.5913 0.044 Uiso 1 1 calc R . . C12 C -0.011(2) 0.7238(14) 0.4142(18) 0.049(7) Uiso 1 1 d G . . H12 H -0.0576 0.7738 0.3636 0.059 Uiso 1 1 calc R . . C13 C 0.062(2) 0.6367(17) 0.3758(18) 0.051(8) Uiso 1 1 d G . . H13 H 0.0727 0.6184 0.2949 0.061 Uiso 1 1 calc R . . C14 C 0.1170(18) 0.5820(14) 0.479(3) 0.12(2) Uani 1 1 d G . . H14 H 0.1703 0.5205 0.4800 0.149 Uiso 1 1 calc R . . C15 C 0.078(2) 0.6352(19) 0.5820(18) 0.12(2) Uani 1 1 d G . . H15 H 0.1005 0.6156 0.6632 0.149 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 0.0239(11) 0.0256(11) 0.0211(11) -0.0005(9) 0.0063(8) -0.0038(9) S2 0.036(3) 0.034(3) 0.023(3) -0.007(3) 0.003(3) -0.001(3) S1 0.040(4) 0.037(3) 0.031(4) 0.003(3) 0.005(3) 0.013(3) C1 0.056(18) 0.029(13) 0.047(17) 0.004(12) 0.026(14) -0.010(12) C2 0.07(2) 0.014(12) 0.07(2) 0.025(13) 0.035(17) 0.012(12) C3 0.060(17) 0.021(12) 0.039(15) -0.008(11) 0.032(13) -0.011(11) S3 0.038(3) 0.036(3) 0.024(3) -0.001(3) 0.010(3) 0.007(3) S4 0.039(3) 0.024(3) 0.025(3) 0.006(3) 0.004(3) 0.003(3) C4 0.066(18) 0.024(12) 0.041(16) -0.007(11) 0.027(14) 0.007(12) C11 0.033(14) 0.027(13) 0.054(18) -0.010(12) 0.022(13) -0.004(10) C14 0.05(2) 0.08(3) 0.26(7) -0.09(4) 0.08(3) -0.05(2) C15 0.06(3) 0.22(6) 0.09(3) 0.02(4) -0.05(2) -0.07(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 Nb1 S1 2.441(7) . y Nb1 S2 2.410(6) . y Nb1 S3 2.420(6) . y Nb1 S4 2.406(6) . y Nb1 C14 2.42(2) . ? Nb1 C15 2.43(2) . ? Nb1 C13 2.45(2) . ? Nb1 C11 2.46(2) . ? Nb1 C12 2.48(2) . ? S2 C3 1.80(3) . y S1 C1 1.80(3) . y C1 C2 1.57(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.54(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? S3 C4 1.83(3) . y S4 C6 1.84(3) . y C4 C5 1.54(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C6 C5 1.52(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C11 C12 1.4200 . ? C11 C15 1.4200 . ? C11 H11 0.9500 . ? C12 C13 1.4200 . ? C12 H12 0.9500 . ? C13 C14 1.4200 . ? C13 H13 0.9500 . ? C14 C15 1.4200 . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? 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 S4 Nb1 S2 79.8(2) . . y S4 Nb1 S3 86.0(2) . . y S2 Nb1 S3 117.3(2) . . y S4 Nb1 C14 79.2(5) . . ? S2 Nb1 C14 132.2(7) . . ? S3 Nb1 C14 103.5(6) . . ? S4 Nb1 C15 81.8(5) . . ? S2 Nb1 C15 100.6(6) . . ? S3 Nb1 C15 137.3(7) . . ? C14 Nb1 C15 34.0(3) . . ? S4 Nb1 S1 152.2(2) . . y S2 Nb1 S1 85.0(2) . . y S3 Nb1 S1 80.5(2) . . y C14 Nb1 S1 127.5(6) . . ? C15 Nb1 S1 124.1(6) . . ? S4 Nb1 C13 109.6(6) . . ? S2 Nb1 C13 151.3(4) . . ? S3 Nb1 C13 90.8(4) . . ? C14 Nb1 C13 33.9(3) . . ? C15 Nb1 C13 56.1(3) . . ? S1 Nb1 C13 94.8(6) . . ? S4 Nb1 C11 113.8(6) . . ? S2 Nb1 C11 95.6(4) . . ? S3 Nb1 C11 144.7(5) . . ? C14 Nb1 C11 56.1(3) . . ? C15 Nb1 C11 33.7(2) . . ? S1 Nb1 C11 90.6(6) . . ? C13 Nb1 C11 55.7(3) . . ? S4 Nb1 C12 133.9(4) . . ? S2 Nb1 C12 121.5(5) . . ? S3 Nb1 C12 112.1(5) . . ? C14 Nb1 C12 55.9(3) . . ? C15 Nb1 C12 55.8(3) . . ? S1 Nb1 C12 73.9(4) . . ? C13 Nb1 C12 33.5(3) . . ? C11 Nb1 C12 33.4(2) . . ? C3 S2 Nb1 111.3(9) . . y C1 S1 Nb1 104.6(10) . . y C2 C1 S1 114.1(16) . . ? C2 C1 H1A 108.7 . . ? S1 C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? S1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C3 C2 C1 111(2) . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C2 C3 S2 115.5(16) . . ? C2 C3 H3A 108.4 . . ? S2 C3 H3A 108.4 . . ? C2 C3 H3B 108.4 . . ? S2 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? C4 S3 Nb1 109.7(8) . . y C6 S4 Nb1 103.2(10) . . y C5 C4 S3 109.0(18) . . ? C5 C4 H4A 109.9 . . ? S3 C4 H4A 109.9 . . ? C5 C4 H4B 109.9 . . ? S3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C5 C6 S4 109(2) . . ? C5 C6 H6A 110.0 . . ? S4 C6 H6A 110.0 . . ? C5 C6 H6B 110.0 . . ? S4 C6 H6B 110.0 . . ? H6A C6 H6B 108.3 . . ? C6 C5 C4 119(2) . . ? C6 C5 H5A 107.7 . . ? C4 C5 H5A 107.7 . . ? C6 C5 H5B 107.7 . . ? C4 C5 H5B 107.7 . . ? H5A C5 H5B 107.1 . . ? C12 C11 C15 108.0 . . ? C12 C11 Nb1 73.8(9) . . ? C15 C11 Nb1 71.9(9) . . ? C12 C11 H11 126.0 . . ? C15 C11 H11 126.0 . . ? Nb1 C11 H11 120.1 . . ? C13 C12 C11 108.0 . . ? C13 C12 Nb1 72.3(8) . . ? C11 C12 Nb1 72.8(8) . . ? C13 C12 H12 126.0 . . ? C11 C12 H12 126.0 . . ? Nb1 C12 H12 120.7 . . ? C12 C13 C14 108.0 . . ? C12 C13 Nb1 74.2(8) . . ? C14 C13 Nb1 72.0(9) . . ? C12 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? Nb1 C13 H13 119.7 . . ? C13 C14 C15 108.0 . . ? C13 C14 Nb1 74.2(9) . . ? C15 C14 Nb1 73.3(8) . . ? C13 C14 H14 126.0 . . ? C15 C14 H14 126.0 . . ? Nb1 C14 H14 118.5 . . ? C14 C15 C11 108.0 . . ? C14 C15 Nb1 72.7(8) . . ? C11 C15 Nb1 74.4(8) . . ? C14 C15 H15 126.0 . . ? C11 C15 H15 126.0 . . ? Nb1 C15 H15 118.8 . . ? 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 S4 Nb1 S2 C3 172.3(8) . . . . ? S3 Nb1 S2 C3 92.3(8) . . . . ? C14 Nb1 S2 C3 -122.5(9) . . . . ? C15 Nb1 S2 C3 -108.2(10) . . . . ? S1 Nb1 S2 C3 15.7(8) . . . . ? C13 Nb1 S2 C3 -75.3(15) . . . . ? C11 Nb1 S2 C3 -74.5(10) . . . . ? C12 Nb1 S2 C3 -51.9(9) . . . . ? S4 Nb1 S1 C1 -12.9(10) . . . . ? S2 Nb1 S1 C1 43.9(8) . . . . ? S3 Nb1 S1 C1 -74.9(8) . . . . ? C14 Nb1 S1 C1 -174.6(11) . . . . ? C15 Nb1 S1 C1 143.3(11) . . . . ? C13 Nb1 S1 C1 -164.9(9) . . . . ? C11 Nb1 S1 C1 139.4(9) . . . . ? C12 Nb1 S1 C1 168.7(10) . . . . ? Nb1 S1 C1 C2 -85.6(19) . . . . ? S1 C1 C2 C3 34(3) . . . . ? C1 C2 C3 S2 50(3) . . . . ? Nb1 S2 C3 C2 -74(2) . . . . ? S4 Nb1 S3 C4 19.8(10) . . . . ? S2 Nb1 S3 C4 96.2(10) . . . . ? C14 Nb1 S3 C4 -58.0(11) . . . . ? C15 Nb1 S3 C4 -53.4(12) . . . . ? S1 Nb1 S3 C4 175.4(10) . . . . ? C13 Nb1 S3 C4 -89.8(11) . . . . ? C11 Nb1 S3 C4 -107.1(13) . . . . ? C12 Nb1 S3 C4 -116.4(11) . . . . ? S2 Nb1 S4 C6 -75.1(10) . . . . ? S3 Nb1 S4 C6 43.5(10) . . . . ? C14 Nb1 S4 C6 148.1(12) . . . . ? C15 Nb1 S4 C6 -177.5(11) . . . . ? S1 Nb1 S4 C6 -17.3(11) . . . . ? C13 Nb1 S4 C6 133.0(10) . . . . ? C11 Nb1 S4 C6 -166.8(10) . . . . ? C12 Nb1 S4 C6 160.6(12) . . . . ? Nb1 S3 C4 C5 -74.4(19) . . . . ? Nb1 S4 C6 C5 -87(2) . . . . ? S4 C6 C5 C4 37(3) . . . . ? S3 C4 C5 C6 47(3) . . . . ? S4 Nb1 C11 C12 -135.1(9) . . . . ? S2 Nb1 C11 C12 143.6(8) . . . . ? S3 Nb1 C11 C12 -15.7(14) . . . . ? S1 Nb1 C11 C12 58.6(9) . . . . ? S4 Nb1 C11 C15 -19.4(10) . . . . ? S2 Nb1 C11 C15 -100.7(9) . . . . ? S3 Nb1 C11 C15 100.0(15) . . . . ? S1 Nb1 C11 C15 174.3(9) . . . . ? C15 C11 C12 C13 0.0 . . . . ? Nb1 C11 C12 C13 64.2(8) . . . . ? C15 C11 C12 Nb1 -64.2(8) . . . . ? S4 Nb1 C12 C13 -52.3(12) . . . . ? S2 Nb1 C12 C13 -159.8(9) . . . . ? S3 Nb1 C12 C13 54.3(8) . . . . ? S1 Nb1 C12 C13 126.7(10) . . . . ? S4 Nb1 C12 C11 63.7(12) . . . . ? S2 Nb1 C12 C11 -43.8(9) . . . . ? S3 Nb1 C12 C11 170.3(8) . . . . ? S1 Nb1 C12 C11 -117.3(10) . . . . ? C11 C12 C13 C14 0.0 . . . . ? Nb1 C12 C13 C14 64.5(9) . . . . ? C11 C12 C13 Nb1 -64.5(9) . . . . ? S4 Nb1 C13 C12 142.8(8) . . . . ? S2 Nb1 C13 C12 37.7(18) . . . . ? S3 Nb1 C13 C12 -131.2(8) . . . . ? S1 Nb1 C13 C12 -50.7(8) . . . . ? S4 Nb1 C13 C14 27.3(9) . . . . ? S2 Nb1 C13 C14 -77.7(19) . . . . ? S3 Nb1 C13 C14 113.4(9) . . . . ? S1 Nb1 C13 C14 -166.1(9) . . . . ? C12 C13 C14 C15 0.0 . . . . ? Nb1 C13 C14 C15 66.0(8) . . . . ? C12 C13 C14 Nb1 -66.0(8) . . . . ? S4 Nb1 C14 C13 -153.9(10) . . . . ? S2 Nb1 C14 C13 140.7(10) . . . . ? S3 Nb1 C14 C13 -70.7(8) . . . . ? S1 Nb1 C14 C13 17.6(12) . . . . ? S4 Nb1 C14 C15 91.2(10) . . . . ? S2 Nb1 C14 C15 25.8(10) . . . . ? S3 Nb1 C14 C15 174.4(8) . . . . ? S1 Nb1 C14 C15 -97.3(13) . . . . ? C13 C14 C15 C11 0.0 . . . . ? Nb1 C14 C15 C11 66.6(9) . . . . ? C13 C14 C15 Nb1 -66.6(9) . . . . ? C12 C11 C15 C14 0.0 . . . . ? Nb1 C11 C15 C14 -65.5(8) . . . . ? C12 C11 C15 Nb1 65.5(8) . . . . ? S4 Nb1 C15 C14 -82.9(10) . . . . ? S2 Nb1 C15 C14 -160.8(9) . . . . ? S3 Nb1 C15 C14 -8.0(12) . . . . ? S1 Nb1 C15 C14 108.1(12) . . . . ? S4 Nb1 C15 C11 162.1(9) . . . . ? S2 Nb1 C15 C11 84.2(8) . . . . ? S3 Nb1 C15 C11 -123.0(11) . . . . ? S1 Nb1 C15 C11 -6.9(12) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 4.546 _refine_diff_density_min -3.098 _refine_diff_density_rms 0.570 #end data_3(194705) _database_code_CSD 194705 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety "(Nb 5+), (C5 H5 1-), (Cl2 1-), (S C2 H4 S C2 H4 S 2-)" _chemical_formula_sum 'C9 H13 Cl2 Nb S3' _chemical_formula_weight 381.18 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' 'S' 'S' 0.1246 0.1234 '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' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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' _cell_length_a 7.9070(10) _cell_length_b 12.4590(10) _cell_length_c 13.1460(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1295.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 15.64 _exptl_crystal_description block _exptl_crystal_colour dark_green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 1.789 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7078 _exptl_absorpt_correction_T_max 0.8047 _exptl_absorpt_process_details 'North et al., 1968' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 1826 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1671 _reflns_number_gt 1567 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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 w1/[\s^2^(Fo^2^)+(0.0331P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(10) _refine_ls_number_reflns 1671 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.91362(5) -0.00204(3) 0.00689(3) 0.01458(14) Uani 1 1 d . . . Cl1 Cl 1.18903(17) -0.05773(11) -0.07144(9) 0.0248(3) Uani 1 1 d . . . Cl2 Cl 0.91827(16) 0.12699(10) -0.13932(9) 0.0204(3) Uani 1 1 d . . . S1 S 0.72591(15) 0.11734(10) 0.10100(10) 0.0178(3) Uani 1 1 d . . . S2 S 1.12678(16) 0.14868(10) 0.05804(10) 0.0173(3) Uani 1 1 d . . . S3 S 1.03676(18) -0.08107(11) 0.16081(10) 0.0235(3) Uani 1 1 d . . . C1 C 0.8470(7) 0.2249(4) 0.1584(4) 0.0202(11) Uani 1 1 d . . . H1A H 0.7731 0.2859 0.1696 0.024 Uiso 1 1 calc R . . H1B H 0.8882 0.2013 0.2242 0.024 Uiso 1 1 calc R . . C2 C 0.9939(6) 0.2599(4) 0.0951(4) 0.0177(11) Uani 1 1 d . . . H2A H 1.0608 0.3112 0.1333 0.021 Uiso 1 1 calc R . . H2B H 0.9523 0.2956 0.0346 0.021 Uiso 1 1 calc R . . C3 C 1.2186(7) 0.1068(4) 0.1786(4) 0.0252(12) Uani 1 1 d . . . H3A H 1.3280 0.1407 0.1879 0.030 Uiso 1 1 calc R . . H3B H 1.1457 0.1284 0.2343 0.030 Uiso 1 1 calc R . . C4 C 1.2387(7) -0.0153(4) 0.1782(4) 0.0253(12) Uani 1 1 d . . . H4A H 1.2884 -0.0383 0.2420 0.030 Uiso 1 1 calc R . . H4B H 1.3147 -0.0360 0.1237 0.030 Uiso 1 1 calc R . . C11 C 0.8212(8) -0.1875(4) 0.0064(5) 0.0362(16) Uani 1 1 d . . . H11 H 0.8874 -0.2394 0.0380 0.043 Uiso 1 1 calc R . . C12 C 0.6936(8) -0.1273(5) 0.0531(5) 0.0333(14) Uani 1 1 d . . . H12 H 0.6603 -0.1315 0.1208 0.040 Uiso 1 1 calc R . . C13 C 0.6250(7) -0.0590(4) -0.0218(5) 0.0316(13) Uani 1 1 d . . . H13 H 0.5381 -0.0097 -0.0124 0.038 Uiso 1 1 calc R . . C14 C 0.7114(7) -0.0788(5) -0.1132(5) 0.0297(13) Uani 1 1 d . . . H14 H 0.6902 -0.0451 -0.1750 0.036 Uiso 1 1 calc R . . C15 C 0.8330(8) -0.1564(5) -0.0966(5) 0.0344(15) Uani 1 1 d . . . H15 H 0.9087 -0.1833 -0.1445 0.041 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 0.0146(2) 0.0124(2) 0.0168(2) 0.00009(19) -0.00126(17) -0.00008(18) Cl1 0.0231(6) 0.0289(7) 0.0226(6) -0.0015(5) 0.0022(5) 0.0089(6) Cl2 0.0219(6) 0.0212(6) 0.0180(5) 0.0041(5) -0.0008(5) 0.0029(6) S1 0.0155(6) 0.0176(6) 0.0203(6) 0.0004(5) 0.0022(5) -0.0009(6) S2 0.0153(6) 0.0172(6) 0.0194(6) 0.0024(5) -0.0016(5) -0.0023(5) S3 0.0271(7) 0.0206(6) 0.0226(6) 0.0083(5) -0.0042(6) -0.0002(6) C1 0.022(3) 0.021(3) 0.018(2) -0.007(2) -0.002(2) -0.002(2) C2 0.019(3) 0.012(2) 0.022(2) 0.000(2) -0.002(2) -0.003(2) C3 0.029(3) 0.023(3) 0.023(3) 0.004(2) -0.015(2) -0.002(3) C4 0.020(3) 0.032(3) 0.025(3) 0.007(2) -0.004(2) -0.001(3) C11 0.038(4) 0.011(2) 0.060(4) -0.003(3) -0.023(4) -0.006(2) C12 0.031(3) 0.028(3) 0.041(3) 0.001(3) -0.003(3) -0.026(3) C13 0.023(3) 0.024(3) 0.048(3) -0.007(3) -0.006(3) -0.011(3) C14 0.032(3) 0.029(3) 0.028(3) -0.007(3) -0.014(3) -0.014(3) C15 0.033(3) 0.026(3) 0.044(3) -0.023(3) -0.007(3) -0.004(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 Nb1 C12 2.415(5) . ? Nb1 C13 2.420(5) . ? Nb1 C11 2.423(5) . ? Nb1 S1 2.4383(13) . y Nb1 C15 2.441(5) . ? Nb1 C14 2.442(5) . ? Nb1 S3 2.4518(13) . y Nb1 Cl2 2.5060(12) . y Nb1 Cl1 2.5068(14) . y Nb1 S2 2.6113(13) . y S1 C1 1.812(5) . y S2 C2 1.806(5) . y S2 C3 1.820(5) . y S3 C4 1.810(5) . y C1 C2 1.494(7) . y C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.529(7) . y C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C11 C12 1.399(9) . ? C11 C15 1.412(10) . ? C11 H11 0.9300 . ? C12 C13 1.410(9) . ? C12 H12 0.9300 . ? C13 C14 1.404(9) . ? C13 H13 0.9300 . ? C14 C15 1.381(9) . ? C14 H14 0.9300 . ? C15 H15 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 C12 Nb1 C13 33.9(2) . . ? C12 Nb1 C11 33.6(2) . . ? C13 Nb1 C11 55.6(2) . . ? C12 Nb1 S1 80.11(16) . . ? C13 Nb1 S1 71.59(15) . . ? C11 Nb1 S1 113.54(17) . . ? C12 Nb1 C15 56.1(2) . . ? C13 Nb1 C15 55.6(2) . . ? C11 Nb1 C15 33.7(2) . . ? S1 Nb1 C15 127.21(16) . . ? C12 Nb1 C14 55.8(2) . . ? C13 Nb1 C14 33.6(2) . . ? C11 Nb1 C14 55.1(2) . . ? S1 Nb1 C14 99.70(15) . . ? C15 Nb1 C14 32.9(2) . . ? C12 Nb1 S3 79.58(16) . . ? C13 Nb1 S3 112.68(15) . . ? C11 Nb1 S3 74.88(16) . . ? S1 Nb1 S3 93.90(5) . . y C15 Nb1 S3 104.32(17) . . ? C14 Nb1 S3 129.51(15) . . ? C12 Nb1 Cl2 128.16(16) . . ? C13 Nb1 Cl2 94.72(15) . . ? C11 Nb1 Cl2 127.88(17) . . ? S1 Nb1 Cl2 90.39(4) . . y C15 Nb1 Cl2 94.69(17) . . ? C14 Nb1 Cl2 76.41(14) . . ? S3 Nb1 Cl2 152.22(5) . . y C12 Nb1 Cl1 123.38(16) . . ? C13 Nb1 Cl1 132.37(15) . . ? C11 Nb1 Cl1 89.82(17) . . ? S1 Nb1 Cl1 154.96(5) . . y C15 Nb1 Cl1 77.27(16) . . ? C14 Nb1 Cl1 101.23(15) . . ? S3 Nb1 Cl1 83.27(5) . . y Cl2 Nb1 Cl1 81.36(4) . . ? C12 Nb1 S2 149.89(16) . . ? C13 Nb1 S2 149.31(14) . . ? C11 Nb1 S2 151.75(15) . . ? S1 Nb1 S2 79.84(4) . . y C15 Nb1 S2 151.49(17) . . ? C14 Nb1 S2 150.54(15) . . ? S3 Nb1 S2 79.63(4) . . y Cl2 Nb1 S2 74.14(4) . . y Cl1 Nb1 S2 75.17(4) . . y C1 S1 Nb1 109.93(18) . . ? C2 S2 C3 102.5(3) . . ? C2 S2 Nb1 104.21(16) . . ? C3 S2 Nb1 106.01(18) . . ? C4 S3 Nb1 105.83(17) . . ? C2 C1 S1 113.2(3) . . y C2 C1 H1A 108.9 . . ? S1 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? S1 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C1 C2 S2 112.3(4) . . y C1 C2 H2A 109.1 . . ? S2 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? S2 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? C4 C3 S2 108.8(4) . . y C4 C3 H3A 109.9 . . ? S2 C3 H3A 109.9 . . ? C4 C3 H3B 109.9 . . ? S2 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C3 C4 S3 111.1(4) . . y C3 C4 H4A 109.4 . . ? S3 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? S3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C12 C11 C15 108.8(6) . . ? C12 C11 Nb1 72.9(3) . . ? C15 C11 Nb1 73.8(3) . . ? C12 C11 H11 125.6 . . ? C15 C11 H11 125.6 . . ? Nb1 C11 H11 119.5 . . ? C11 C12 C13 107.1(6) . . ? C11 C12 Nb1 73.5(3) . . ? C13 C12 Nb1 73.3(3) . . ? C11 C12 H12 126.4 . . ? C13 C12 H12 126.4 . . ? Nb1 C12 H12 118.8 . . ? C14 C13 C12 107.7(6) . . ? C14 C13 Nb1 74.1(3) . . ? C12 C13 Nb1 72.8(3) . . ? C14 C13 H13 126.1 . . ? C12 C13 H13 126.1 . . ? Nb1 C13 H13 118.8 . . ? C15 C14 C13 109.1(5) . . ? C15 C14 Nb1 73.5(3) . . ? C13 C14 Nb1 72.3(3) . . ? C15 C14 H14 125.5 . . ? C13 C14 H14 125.5 . . ? Nb1 C14 H14 120.4 . . ? C14 C15 C11 107.3(6) . . ? C14 C15 Nb1 73.6(3) . . ? C11 C15 Nb1 72.4(3) . . ? C14 C15 H15 126.4 . . ? C11 C15 H15 126.4 . . ? Nb1 C15 H15 119.5 . . ? 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 C12 Nb1 S1 C1 151.3(2) . . . . ? C13 Nb1 S1 C1 -174.7(2) . . . . ? C11 Nb1 S1 C1 147.8(2) . . . . ? C15 Nb1 S1 C1 -176.1(3) . . . . ? C14 Nb1 S1 C1 -156.2(2) . . . . ? S3 Nb1 S1 C1 72.63(18) . . . . ? Cl2 Nb1 S1 C1 -79.90(19) . . . . ? Cl1 Nb1 S1 C1 -9.8(2) . . . . ? S2 Nb1 S1 C1 -6.09(18) . . . . ? C12 Nb1 S2 C2 -65.2(4) . . . . ? C13 Nb1 S2 C2 5.1(4) . . . . ? C11 Nb1 S2 C2 -137.9(4) . . . . ? S1 Nb1 S2 C2 -16.30(18) . . . . ? C15 Nb1 S2 C2 146.8(4) . . . . ? C14 Nb1 S2 C2 75.5(3) . . . . ? S3 Nb1 S2 C2 -112.21(18) . . . . ? Cl2 Nb1 S2 C2 77.03(18) . . . . ? Cl1 Nb1 S2 C2 162.07(18) . . . . ? C12 Nb1 S2 C3 42.6(4) . . . . ? C13 Nb1 S2 C3 112.9(3) . . . . ? C11 Nb1 S2 C3 -30.1(4) . . . . ? S1 Nb1 S2 C3 91.5(2) . . . . ? C15 Nb1 S2 C3 -105.4(4) . . . . ? C14 Nb1 S2 C3 -176.8(3) . . . . ? S3 Nb1 S2 C3 -4.4(2) . . . . ? Cl2 Nb1 S2 C3 -175.2(2) . . . . ? Cl1 Nb1 S2 C3 -90.2(2) . . . . ? C12 Nb1 S3 C4 -179.9(3) . . . . ? C13 Nb1 S3 C4 -172.4(3) . . . . ? C11 Nb1 S3 C4 146.0(3) . . . . ? S1 Nb1 S3 C4 -100.7(2) . . . . ? C15 Nb1 S3 C4 129.3(3) . . . . ? C14 Nb1 S3 C4 153.3(3) . . . . ? Cl2 Nb1 S3 C4 -2.4(2) . . . . ? Cl1 Nb1 S3 C4 54.3(2) . . . . ? S2 Nb1 S3 C4 -21.8(2) . . . . ? Nb1 S1 C1 C2 34.4(4) . . . . ? S1 C1 C2 S2 -52.1(5) . . . . ? C3 S2 C2 C1 -67.8(4) . . . . ? Nb1 S2 C2 C1 42.5(4) . . . . ? C2 S2 C3 C4 144.7(4) . . . . ? Nb1 S2 C3 C4 35.8(4) . . . . ? S2 C3 C4 S3 -59.5(5) . . . . ? Nb1 S3 C4 C3 53.4(4) . . . . ? C13 Nb1 C11 C12 -38.1(4) . . . . ? S1 Nb1 C11 C12 6.3(4) . . . . ? C15 Nb1 C11 C12 -116.1(6) . . . . ? C14 Nb1 C11 C12 -79.1(4) . . . . ? S3 Nb1 C11 C12 93.9(4) . . . . ? Cl2 Nb1 C11 C12 -104.1(4) . . . . ? Cl1 Nb1 C11 C12 177.0(4) . . . . ? S2 Nb1 C11 C12 120.1(4) . . . . ? C12 Nb1 C11 C15 116.1(6) . . . . ? C13 Nb1 C11 C15 78.0(4) . . . . ? S1 Nb1 C11 C15 122.4(4) . . . . ? C14 Nb1 C11 C15 37.0(4) . . . . ? S3 Nb1 C11 C15 -150.0(4) . . . . ? Cl2 Nb1 C11 C15 12.0(5) . . . . ? Cl1 Nb1 C11 C15 -66.9(4) . . . . ? S2 Nb1 C11 C15 -123.8(4) . . . . ? C15 C11 C12 C13 0.4(6) . . . . ? Nb1 C11 C12 C13 66.1(4) . . . . ? C15 C11 C12 Nb1 -65.6(4) . . . . ? C13 Nb1 C12 C11 114.2(6) . . . . ? S1 Nb1 C12 C11 -174.2(4) . . . . ? C15 Nb1 C12 C11 36.9(4) . . . . ? C14 Nb1 C12 C11 76.8(4) . . . . ? S3 Nb1 C12 C11 -78.3(4) . . . . ? Cl2 Nb1 C12 C11 103.2(4) . . . . ? Cl1 Nb1 C12 C11 -3.6(5) . . . . ? S2 Nb1 C12 C11 -125.3(4) . . . . ? C11 Nb1 C12 C13 -114.2(6) . . . . ? S1 Nb1 C12 C13 71.6(4) . . . . ? C15 Nb1 C12 C13 -77.3(4) . . . . ? C14 Nb1 C12 C13 -37.4(4) . . . . ? S3 Nb1 C12 C13 167.5(4) . . . . ? Cl2 Nb1 C12 C13 -11.0(5) . . . . ? Cl1 Nb1 C12 C13 -117.8(3) . . . . ? S2 Nb1 C12 C13 120.5(4) . . . . ? C11 C12 C13 C14 0.2(6) . . . . ? Nb1 C12 C13 C14 66.4(4) . . . . ? C11 C12 C13 Nb1 -66.3(4) . . . . ? C12 Nb1 C13 C14 -114.8(5) . . . . ? C11 Nb1 C13 C14 -77.1(4) . . . . ? S1 Nb1 C13 C14 145.4(4) . . . . ? C15 Nb1 C13 C14 -35.9(4) . . . . ? S3 Nb1 C13 C14 -128.1(3) . . . . ? Cl2 Nb1 C13 C14 56.6(3) . . . . ? Cl1 Nb1 C13 C14 -26.0(4) . . . . ? S2 Nb1 C13 C14 123.1(3) . . . . ? C11 Nb1 C13 C12 37.7(4) . . . . ? S1 Nb1 C13 C12 -99.8(4) . . . . ? C15 Nb1 C13 C12 78.9(4) . . . . ? C14 Nb1 C13 C12 114.8(5) . . . . ? S3 Nb1 C13 C12 -13.3(4) . . . . ? Cl2 Nb1 C13 C12 171.3(4) . . . . ? Cl1 Nb1 C13 C12 88.7(4) . . . . ? S2 Nb1 C13 C12 -122.1(4) . . . . ? C12 C13 C14 C15 -0.8(6) . . . . ? Nb1 C13 C14 C15 64.8(4) . . . . ? C12 C13 C14 Nb1 -65.6(4) . . . . ? C12 Nb1 C14 C15 -79.1(4) . . . . ? C13 Nb1 C14 C15 -116.9(5) . . . . ? C11 Nb1 C14 C15 -38.0(4) . . . . ? S1 Nb1 C14 C15 -150.0(4) . . . . ? S3 Nb1 C14 C15 -46.7(4) . . . . ? Cl2 Nb1 C14 C15 122.0(4) . . . . ? Cl1 Nb1 C14 C15 43.8(4) . . . . ? S2 Nb1 C14 C15 123.5(4) . . . . ? C12 Nb1 C14 C13 37.8(4) . . . . ? C11 Nb1 C14 C13 78.9(4) . . . . ? S1 Nb1 C14 C13 -33.1(4) . . . . ? C15 Nb1 C14 C13 116.9(5) . . . . ? S3 Nb1 C14 C13 70.2(4) . . . . ? Cl2 Nb1 C14 C13 -121.2(4) . . . . ? Cl1 Nb1 C14 C13 160.7(3) . . . . ? S2 Nb1 C14 C13 -119.6(4) . . . . ? C13 C14 C15 C11 1.0(6) . . . . ? Nb1 C14 C15 C11 65.1(4) . . . . ? C13 C14 C15 Nb1 -64.1(4) . . . . ? C12 C11 C15 C14 -0.9(6) . . . . ? Nb1 C11 C15 C14 -65.9(4) . . . . ? C12 C11 C15 Nb1 65.0(4) . . . . ? C12 Nb1 C15 C14 77.9(4) . . . . ? C13 Nb1 C15 C14 36.7(4) . . . . ? C11 Nb1 C15 C14 114.7(6) . . . . ? S1 Nb1 C15 C14 38.2(4) . . . . ? S3 Nb1 C15 C14 144.6(3) . . . . ? Cl2 Nb1 C15 C14 -55.8(4) . . . . ? Cl1 Nb1 C15 C14 -135.9(4) . . . . ? S2 Nb1 C15 C14 -120.8(4) . . . . ? C12 Nb1 C15 C11 -36.8(4) . . . . ? C13 Nb1 C15 C11 -78.0(4) . . . . ? S1 Nb1 C15 C11 -76.5(4) . . . . ? C14 Nb1 C15 C11 -114.7(6) . . . . ? S3 Nb1 C15 C11 29.9(4) . . . . ? Cl2 Nb1 C15 C11 -170.5(4) . . . . ? Cl1 Nb1 C15 C11 109.4(4) . . . . ? S2 Nb1 C15 C11 124.5(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.380 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.105 #END data_5(194706) _database_code_CSD 194706 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety "(Nb 5+), (C6 H7 1-), (Cl 1-)2, (S2 C4 H8 O 2-)" _chemical_formula_sum 'C10 H15 Cl2 Nb O S2' _chemical_formula_weight 379.15 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' 'O' 'O' 0.0106 0.0060 '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' 'Cl' 'Cl' 0.1484 0.1585 '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 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 14.3244(11) _cell_length_b 12.0161(11) _cell_length_c 7.8488(8) _cell_angle_alpha 90.00 _cell_angle_beta 104.510(9) _cell_angle_gamma 90.00 _cell_volume 1307.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 4.83 _cell_measurement_theta_max 12.58 _exptl_crystal_description lozenge _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.926 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 1.623 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.4746 _exptl_absorpt_correction_T_max 0.5752 _exptl_absorpt_process_details 'North et al., 1968' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3062 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2257 _reflns_number_gt 1670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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 w1/[\s^2^(Fo^2^)+(0.0551P)^2^+6.1860P] 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 2257 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1340 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 0.26438(3) 0.50099(3) 0.65414(6) 0.0128(2) Uani 1 1 d . . . Cl1 Cl 0.34085(10) 0.49022(11) 0.97691(17) 0.0227(3) Uani 1 1 d . . . Cl2 Cl 0.12297(9) 0.50574(10) 0.38874(17) 0.0206(3) Uani 1 1 d . . . O1 O 0.1364(3) 0.5002(3) 0.7707(5) 0.0162(8) Uani 1 1 d . . . S1 S 0.23696(10) 0.69813(11) 0.68892(18) 0.0203(3) Uani 1 1 d . . . S2 S 0.22876(9) 0.30418(11) 0.66486(18) 0.0191(3) Uani 1 1 d . . . C1 C 0.1211(4) 0.6970(5) 0.7464(8) 0.0249(13) Uani 1 1 d . . . H1A H 0.1136 0.7669 0.8086 0.030 Uiso 1 1 calc R . . H1B H 0.0682 0.6931 0.6378 0.030 Uiso 1 1 calc R . . C2 C 0.1148(4) 0.5986(4) 0.8630(7) 0.0216(12) Uani 1 1 d . . . H2A H 0.1620 0.6063 0.9785 0.026 Uiso 1 1 calc R . . H2B H 0.0493 0.5930 0.8827 0.026 Uiso 1 1 calc R . . C3 C 0.1113(4) 0.3990(4) 0.8493(7) 0.0188(11) Uani 1 1 d . . . H3A H 0.0460 0.4056 0.8692 0.023 Uiso 1 1 calc R . . H3B H 0.1578 0.3853 0.9640 0.023 Uiso 1 1 calc R . . C4 C 0.1142(4) 0.3055(5) 0.7251(7) 0.0210(12) Uani 1 1 d . . . H4A H 0.0609 0.3140 0.6179 0.025 Uiso 1 1 calc R . . H4B H 0.1053 0.2339 0.7814 0.025 Uiso 1 1 calc R . . C11 C 0.4178(4) 0.4198(5) 0.6327(8) 0.0232(12) Uani 1 1 d . . . C12 C 0.3555(4) 0.4187(5) 0.4619(8) 0.0263(13) Uani 1 1 d . . . H12 H 0.3321 0.3541 0.3948 0.032 Uiso 1 1 calc R . . C13 C 0.3339(4) 0.5292(5) 0.4079(8) 0.0234(12) Uani 1 1 d . . . H13 H 0.2925 0.5522 0.2992 0.028 Uiso 1 1 calc R . . C14 C 0.3842(4) 0.5998(5) 0.5431(8) 0.0249(13) Uani 1 1 d . . . H14 H 0.3835 0.6788 0.5410 0.030 Uiso 1 1 calc R . . C15 C 0.4357(4) 0.5324(5) 0.6822(8) 0.0232(12) Uani 1 1 d . . . H15 H 0.4755 0.5582 0.7906 0.028 Uiso 1 1 calc R . . C16 C 0.4645(5) 0.3202(5) 0.7363(10) 0.0382(17) Uani 1 1 d . . . H16A H 0.5325 0.3168 0.7342 0.057 Uiso 1 1 calc R . . H16B H 0.4315 0.2523 0.6839 0.057 Uiso 1 1 calc R . . H16C H 0.4597 0.3269 0.8583 0.057 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 0.0091(3) 0.0115(3) 0.0152(3) -0.00047(17) -0.00165(19) -0.00018(16) Cl1 0.0151(7) 0.0328(8) 0.0165(6) 0.0012(5) -0.0031(5) 0.0020(5) Cl2 0.0146(6) 0.0199(7) 0.0217(7) 0.0003(5) -0.0057(5) -0.0003(5) O1 0.0131(19) 0.0152(19) 0.0182(18) -0.0022(14) 0.0003(14) -0.0004(13) S1 0.0193(7) 0.0118(6) 0.0279(7) -0.0014(5) 0.0020(6) -0.0005(5) S2 0.0160(7) 0.0120(6) 0.0272(7) 0.0005(5) 0.0016(5) 0.0002(5) C1 0.015(3) 0.020(3) 0.037(3) 0.000(2) 0.003(2) 0.003(2) C2 0.022(3) 0.017(3) 0.023(3) -0.001(2) 0.001(2) 0.003(2) C3 0.016(3) 0.017(3) 0.021(3) 0.008(2) 0.001(2) -0.001(2) C4 0.014(3) 0.021(3) 0.026(3) 0.003(2) 0.000(2) -0.005(2) C11 0.011(2) 0.026(3) 0.033(3) 0.010(2) 0.007(2) 0.006(2) C12 0.017(3) 0.027(3) 0.036(3) -0.014(3) 0.009(2) -0.001(2) C13 0.014(3) 0.032(3) 0.025(3) 0.009(2) 0.005(2) 0.003(2) C14 0.015(3) 0.022(3) 0.038(3) -0.002(3) 0.007(2) -0.007(2) C15 0.010(3) 0.032(3) 0.027(3) -0.002(3) 0.003(2) -0.004(2) C16 0.020(3) 0.033(4) 0.066(5) 0.021(3) 0.018(3) 0.014(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 Nb1 O1 2.245(4) . y Nb1 C13 2.409(6) . ? Nb1 C14 2.421(5) . ? Nb1 S2 2.4252(14) . y Nb1 S1 2.4278(14) . y Nb1 C12 2.438(6) . ? Nb1 C15 2.438(5) . ? Nb1 C11 2.449(5) . ? Nb1 Cl1 2.4988(13) . y Nb1 Cl2 2.5162(13) . y O1 C3 1.448(6) . y O1 C2 1.459(6) . y S1 C1 1.825(6) . y S2 C4 1.818(6) . y C1 C2 1.512(8) . y C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.495(8) . y C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C11 C12 1.413(8) . ? C11 C15 1.413(8) . ? C11 C16 1.505(8) . ? C12 C13 1.404(8) . ? C12 H12 0.9500 . ? C13 C14 1.408(8) . ? C13 H13 0.9500 . ? C14 C15 1.410(8) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 O1 Nb1 C13 150.61(16) . . ? O1 Nb1 C14 150.89(16) . . ? C13 Nb1 C14 33.9(2) . . ? O1 Nb1 S2 77.36(9) . . y C13 Nb1 S2 107.32(15) . . ? C14 Nb1 S2 131.67(14) . . ? O1 Nb1 S1 77.69(9) . . y C13 Nb1 S1 93.67(15) . . ? C14 Nb1 S1 73.22(14) . . ? S2 Nb1 S1 154.98(5) . . y O1 Nb1 C12 150.33(16) . . ? C13 Nb1 C12 33.7(2) . . ? C14 Nb1 C12 55.9(2) . . ? S2 Nb1 C12 77.04(15) . . ? S1 Nb1 C12 126.31(15) . . ? O1 Nb1 C15 150.50(17) . . ? C13 Nb1 C15 56.07(19) . . ? C14 Nb1 C15 33.73(19) . . ? S2 Nb1 C15 111.32(15) . . ? S1 Nb1 C15 91.51(15) . . ? C12 Nb1 C15 55.7(2) . . ? O1 Nb1 C11 149.89(16) . . ? C13 Nb1 C11 56.12(19) . . ? C14 Nb1 C11 56.04(19) . . ? S2 Nb1 C11 79.29(14) . . ? S1 Nb1 C11 124.74(14) . . ? C12 Nb1 C11 33.6(2) . . ? C15 Nb1 C11 33.63(19) . . ? O1 Nb1 Cl1 77.40(10) . . y C13 Nb1 Cl1 131.02(14) . . ? C14 Nb1 Cl1 102.71(15) . . ? S2 Nb1 Cl1 87.53(5) . . y S1 Nb1 Cl1 88.78(5) . . y C12 Nb1 Cl1 116.09(15) . . ? C15 Nb1 Cl1 74.97(14) . . ? C11 Nb1 Cl1 82.88(14) . . ? O1 Nb1 Cl2 76.54(10) . . y C13 Nb1 Cl2 75.01(14) . . ? C14 Nb1 Cl2 100.78(14) . . ? S2 Nb1 Cl2 85.30(4) . . y S1 Nb1 Cl2 87.22(4) . . y C12 Nb1 Cl2 86.64(15) . . ? C15 Nb1 Cl2 130.89(14) . . ? C11 Nb1 Cl2 120.16(14) . . ? Cl1 Nb1 Cl2 153.90(5) . . ? C3 O1 C2 111.3(4) . . y C3 O1 Nb1 119.5(3) . . y C2 O1 Nb1 119.7(3) . . y C1 S1 Nb1 101.74(19) . . y C4 S2 Nb1 102.24(18) . . y C2 C1 S1 110.6(4) . . y C2 C1 H1A 109.5 . . ? S1 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? O1 C2 C1 106.3(4) . . y O1 C2 H2A 110.5 . . ? C1 C2 H2A 110.5 . . ? O1 C2 H2B 110.5 . . ? C1 C2 H2B 110.5 . . ? H2A C2 H2B 108.7 . . ? O1 C3 C4 107.6(4) . . y O1 C3 H3A 110.2 . . ? C4 C3 H3A 110.2 . . ? O1 C3 H3B 110.2 . . ? C4 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? C3 C4 S2 110.5(4) . . y C3 C4 H4A 109.5 . . ? S2 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? S2 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C12 C11 C15 107.3(5) . . ? C12 C11 C16 126.5(6) . . ? C15 C11 C16 125.9(6) . . ? C12 C11 Nb1 72.8(3) . . ? C15 C11 Nb1 72.7(3) . . ? C16 C11 Nb1 124.3(4) . . ? C13 C12 C11 108.4(5) . . ? C13 C12 Nb1 72.0(3) . . ? C11 C12 Nb1 73.6(3) . . ? C13 C12 H12 125.8 . . ? C11 C12 H12 125.8 . . ? Nb1 C12 H12 120.3 . . ? C12 C13 C14 108.1(5) . . ? C12 C13 Nb1 74.3(3) . . ? C14 C13 Nb1 73.5(3) . . ? C12 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? Nb1 C13 H13 118.1 . . ? C13 C14 C15 107.9(5) . . ? C13 C14 Nb1 72.6(3) . . ? C15 C14 Nb1 73.8(3) . . ? C13 C14 H14 126.1 . . ? C15 C14 H14 126.1 . . ? Nb1 C14 H14 119.5 . . ? C14 C15 C11 108.3(5) . . ? C14 C15 Nb1 72.5(3) . . ? C11 C15 Nb1 73.6(3) . . ? C14 C15 H15 125.9 . . ? C11 C15 H15 125.9 . . ? Nb1 C15 H15 119.8 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 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 C13 Nb1 O1 C3 122.1(4) . . . . ? C14 Nb1 O1 C3 -164.6(4) . . . . ? S2 Nb1 O1 C3 19.2(3) . . . . ? S1 Nb1 O1 C3 -162.6(3) . . . . ? C12 Nb1 O1 C3 50.1(5) . . . . ? C15 Nb1 O1 C3 -91.9(5) . . . . ? C11 Nb1 O1 C3 -20.8(5) . . . . ? Cl1 Nb1 O1 C3 -71.1(3) . . . . ? Cl2 Nb1 O1 C3 107.3(3) . . . . ? C13 Nb1 O1 C2 -94.6(5) . . . . ? C14 Nb1 O1 C2 -21.4(5) . . . . ? S2 Nb1 O1 C2 162.4(3) . . . . ? S1 Nb1 O1 C2 -19.3(3) . . . . ? C12 Nb1 O1 C2 -166.6(4) . . . . ? C15 Nb1 O1 C2 51.3(5) . . . . ? C11 Nb1 O1 C2 122.5(4) . . . . ? Cl1 Nb1 O1 C2 72.2(3) . . . . ? Cl2 Nb1 O1 C2 -109.4(3) . . . . ? O1 Nb1 S1 C1 -9.6(2) . . . . ? C13 Nb1 S1 C1 142.0(2) . . . . ? C14 Nb1 S1 C1 169.4(2) . . . . ? S2 Nb1 S1 C1 -5.4(2) . . . . ? C12 Nb1 S1 C1 151.0(3) . . . . ? C15 Nb1 S1 C1 -161.9(2) . . . . ? C11 Nb1 S1 C1 -167.4(3) . . . . ? Cl1 Nb1 S1 C1 -87.0(2) . . . . ? Cl2 Nb1 S1 C1 67.2(2) . . . . ? O1 Nb1 S2 C4 8.9(2) . . . . ? C13 Nb1 S2 C4 -141.0(2) . . . . ? C14 Nb1 S2 C4 -168.6(3) . . . . ? S1 Nb1 S2 C4 4.7(2) . . . . ? C12 Nb1 S2 C4 -156.0(2) . . . . ? C15 Nb1 S2 C4 159.3(2) . . . . ? C11 Nb1 S2 C4 169.7(2) . . . . ? Cl1 Nb1 S2 C4 86.53(19) . . . . ? Cl2 Nb1 S2 C4 -68.35(18) . . . . ? Nb1 S1 C1 C2 37.1(4) . . . . ? C3 O1 C2 C1 -166.9(4) . . . . ? Nb1 O1 C2 C1 47.1(5) . . . . ? S1 C1 C2 O1 -53.5(5) . . . . ? C2 O1 C3 C4 167.3(4) . . . . ? Nb1 O1 C3 C4 -46.6(5) . . . . ? O1 C3 C4 S2 52.3(5) . . . . ? Nb1 S2 C4 C3 -35.6(4) . . . . ? O1 Nb1 C11 C12 122.3(4) . . . . ? C13 Nb1 C11 C12 -36.8(3) . . . . ? C14 Nb1 C11 C12 -77.9(4) . . . . ? S2 Nb1 C11 C12 82.7(3) . . . . ? S1 Nb1 C11 C12 -105.0(4) . . . . ? C15 Nb1 C11 C12 -115.0(5) . . . . ? Cl1 Nb1 C11 C12 171.5(4) . . . . ? Cl2 Nb1 C11 C12 4.6(4) . . . . ? O1 Nb1 C11 C15 -122.7(4) . . . . ? C13 Nb1 C11 C15 78.2(4) . . . . ? C14 Nb1 C11 C15 37.1(3) . . . . ? S2 Nb1 C11 C15 -162.3(3) . . . . ? S1 Nb1 C11 C15 10.0(4) . . . . ? C12 Nb1 C11 C15 115.0(5) . . . . ? Cl1 Nb1 C11 C15 -73.5(3) . . . . ? Cl2 Nb1 C11 C15 119.6(3) . . . . ? O1 Nb1 C11 C16 -0.5(8) . . . . ? C13 Nb1 C11 C16 -159.7(6) . . . . ? C14 Nb1 C11 C16 159.2(6) . . . . ? S2 Nb1 C11 C16 -40.2(5) . . . . ? S1 Nb1 C11 C16 132.2(5) . . . . ? C12 Nb1 C11 C16 -122.8(7) . . . . ? C15 Nb1 C11 C16 122.1(7) . . . . ? Cl1 Nb1 C11 C16 48.6(5) . . . . ? Cl2 Nb1 C11 C16 -118.3(5) . . . . ? C15 C11 C12 C13 -1.0(7) . . . . ? C16 C11 C12 C13 -175.6(5) . . . . ? Nb1 C11 C12 C13 64.1(4) . . . . ? C15 C11 C12 Nb1 -65.0(4) . . . . ? C16 C11 C12 Nb1 120.3(6) . . . . ? O1 Nb1 C12 C13 122.7(4) . . . . ? C14 Nb1 C12 C13 -37.7(3) . . . . ? S2 Nb1 C12 C13 153.7(3) . . . . ? S1 Nb1 C12 C13 -16.4(4) . . . . ? C15 Nb1 C12 C13 -78.8(4) . . . . ? C11 Nb1 C12 C13 -116.2(5) . . . . ? Cl1 Nb1 C12 C13 -125.6(3) . . . . ? Cl2 Nb1 C12 C13 67.7(3) . . . . ? O1 Nb1 C12 C11 -121.1(4) . . . . ? C13 Nb1 C12 C11 116.2(5) . . . . ? C14 Nb1 C12 C11 78.5(4) . . . . ? S2 Nb1 C12 C11 -90.1(3) . . . . ? S1 Nb1 C12 C11 99.9(4) . . . . ? C15 Nb1 C12 C11 37.4(3) . . . . ? Cl1 Nb1 C12 C11 -9.4(4) . . . . ? Cl2 Nb1 C12 C11 -176.0(3) . . . . ? C11 C12 C13 C14 1.2(7) . . . . ? Nb1 C12 C13 C14 66.3(4) . . . . ? C11 C12 C13 Nb1 -65.1(4) . . . . ? O1 Nb1 C13 C12 -121.9(4) . . . . ? C14 Nb1 C13 C12 114.8(5) . . . . ? S2 Nb1 C13 C12 -26.9(3) . . . . ? S1 Nb1 C13 C12 166.9(3) . . . . ? C15 Nb1 C13 C12 77.5(4) . . . . ? C11 Nb1 C13 C12 36.7(3) . . . . ? Cl1 Nb1 C13 C12 75.3(4) . . . . ? Cl2 Nb1 C13 C12 -107.0(3) . . . . ? O1 Nb1 C13 C14 123.3(4) . . . . ? S2 Nb1 C13 C14 -141.7(3) . . . . ? S1 Nb1 C13 C14 52.1(3) . . . . ? C12 Nb1 C13 C14 -114.8(5) . . . . ? C15 Nb1 C13 C14 -37.3(3) . . . . ? C11 Nb1 C13 C14 -78.0(4) . . . . ? Cl1 Nb1 C13 C14 -39.5(4) . . . . ? Cl2 Nb1 C13 C14 138.2(3) . . . . ? C12 C13 C14 C15 -1.0(6) . . . . ? Nb1 C13 C14 C15 65.9(4) . . . . ? C12 C13 C14 Nb1 -66.8(4) . . . . ? O1 Nb1 C14 C13 -122.6(4) . . . . ? S2 Nb1 C14 C13 52.4(4) . . . . ? S1 Nb1 C14 C13 -124.7(3) . . . . ? C12 Nb1 C14 C13 37.5(3) . . . . ? C15 Nb1 C14 C13 115.3(5) . . . . ? C11 Nb1 C14 C13 78.3(4) . . . . ? Cl1 Nb1 C14 C13 150.5(3) . . . . ? Cl2 Nb1 C14 C13 -40.9(3) . . . . ? O1 Nb1 C14 C15 122.2(4) . . . . ? C13 Nb1 C14 C15 -115.3(5) . . . . ? S2 Nb1 C14 C15 -62.9(4) . . . . ? S1 Nb1 C14 C15 120.1(3) . . . . ? C12 Nb1 C14 C15 -77.8(4) . . . . ? C11 Nb1 C14 C15 -37.0(3) . . . . ? Cl1 Nb1 C14 C15 35.3(3) . . . . ? Cl2 Nb1 C14 C15 -156.2(3) . . . . ? C13 C14 C15 C11 0.4(6) . . . . ? Nb1 C14 C15 C11 65.5(4) . . . . ? C13 C14 C15 Nb1 -65.1(4) . . . . ? C12 C11 C15 C14 0.3(6) . . . . ? C16 C11 C15 C14 175.0(5) . . . . ? Nb1 C11 C15 C14 -64.7(4) . . . . ? C12 C11 C15 Nb1 65.1(4) . . . . ? C16 C11 C15 Nb1 -120.3(6) . . . . ? O1 Nb1 C15 C14 -123.2(4) . . . . ? C13 Nb1 C15 C14 37.4(3) . . . . ? S2 Nb1 C15 C14 134.5(3) . . . . ? S1 Nb1 C15 C14 -56.0(3) . . . . ? C12 Nb1 C15 C14 78.4(4) . . . . ? C11 Nb1 C15 C14 115.8(5) . . . . ? Cl1 Nb1 C15 C14 -144.3(4) . . . . ? Cl2 Nb1 C15 C14 31.7(4) . . . . ? O1 Nb1 C15 C11 121.0(4) . . . . ? C13 Nb1 C15 C11 -78.4(4) . . . . ? C14 Nb1 C15 C11 -115.8(5) . . . . ? S2 Nb1 C15 C11 18.7(4) . . . . ? S1 Nb1 C15 C11 -171.8(3) . . . . ? C12 Nb1 C15 C11 -37.4(3) . . . . ? Cl1 Nb1 C15 C11 99.9(3) . . . . ? Cl2 Nb1 C15 C11 -84.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.084 _refine_diff_density_min -1.075 _refine_diff_density_rms 0.158 #end data_6(194707) _database_code_CSD 194707 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety "(Nb 5+), (C6 H7 1-), (O 2-), (S2 C4 H8 O 2-)" _chemical_formula_sum 'C10 H15 Nb O2 S2' _chemical_formula_weight 324.25 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' 'S' 'S' 0.1246 0.1234 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.695(2) _cell_length_b 13.098(3) _cell_length_c 13.984(3) _cell_angle_alpha 64.180(10) _cell_angle_beta 75.090(10) _cell_angle_gamma 87.720(10) _cell_volume 1221.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 5.29 _cell_measurement_theta_max 12.48 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 1.304 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7515 _exptl_absorpt_correction_T_max 0.9201 _exptl_absorpt_process_details 'North et al., 1968' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5044 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4082 _reflns_number_gt 3462 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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 w1/[\s^2^(Fo^2^)+(0.0510P)^2^+1.1472P] 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 4082 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.38006(5) 1.00355(3) 0.24853(3) 0.01856(13) Uani 1 1 d . . . O1 O 0.4920(5) 1.1170(3) 0.1261(3) 0.0343(8) Uani 1 1 d . . . S1 S 0.56956(16) 0.84354(11) 0.26115(11) 0.0340(3) Uani 1 1 d . . . O11 O 0.2825(4) 0.9204(3) 0.1505(2) 0.0265(7) Uani 1 1 d . . . S2 S 0.05498(16) 1.03270(11) 0.26995(11) 0.0329(3) Uani 1 1 d . . . C1 C 0.5608(7) 0.8360(4) 0.1360(4) 0.0357(11) Uani 1 1 d . . . H1A H 0.6255 0.9051 0.0711 0.043 Uiso 1 1 calc R . . H1B H 0.6213 0.7691 0.1325 0.043 Uiso 1 1 calc R . . C2 C 0.3692(7) 0.8264(4) 0.1338(4) 0.0325(11) Uani 1 1 d . . . H2A H 0.3641 0.8309 0.0621 0.039 Uiso 1 1 calc R . . H2B H 0.3074 0.7528 0.1931 0.039 Uiso 1 1 calc R . . C3 C 0.0999(7) 0.9219(4) 0.1417(4) 0.0320(11) Uani 1 1 d . . . H3A H 0.0258 0.8535 0.2027 0.038 Uiso 1 1 calc R . . H3B H 0.0978 0.9224 0.0710 0.038 Uiso 1 1 calc R . . C4 C 0.0264(7) 1.0275(4) 0.1473(4) 0.0329(11) Uani 1 1 d . . . H4A H -0.1032 1.0274 0.1495 0.040 Uiso 1 1 calc R . . H4B H 0.0910 1.0956 0.0809 0.040 Uiso 1 1 calc R . . C11 C 0.5075(6) 1.1070(4) 0.3294(4) 0.0238(9) Uani 1 1 d . . . C12 C 0.3171(6) 1.0990(4) 0.3682(4) 0.0258(10) Uani 1 1 d . . . H12 H 0.2421 1.1602 0.3493 0.031 Uiso 1 1 calc R . . C13 C 0.2573(6) 0.9810(4) 0.4416(4) 0.0272(10) Uani 1 1 d . . . H13 H 0.1365 0.9516 0.4824 0.033 Uiso 1 1 calc R . . C14 C 0.4051(6) 0.9188(4) 0.4421(4) 0.0267(10) Uani 1 1 d . . . H14 H 0.4043 0.8388 0.4830 0.032 Uiso 1 1 calc R . . C15 C 0.5610(6) 0.9957(4) 0.3703(3) 0.0247(9) Uani 1 1 d . . . H15 H 0.6806 0.9748 0.3533 0.030 Uiso 1 1 calc R . . C16 C 0.6279(7) 1.2138(4) 0.2551(4) 0.0347(11) Uani 1 1 d . . . H16A H 0.7319 1.2132 0.2836 0.052 Uiso 1 1 calc R . . H16B H 0.5607 1.2798 0.2521 0.052 Uiso 1 1 calc R . . H16C H 0.6699 1.2183 0.1809 0.052 Uiso 1 1 calc R . . Nb2 Nb 0.14772(5) 0.47599(3) 0.26304(3) 0.01759(12) Uani 1 1 d . . . O2 O 0.0559(4) 0.5911(3) 0.2820(2) 0.0255(7) Uani 1 1 d . . . S3 S 0.47799(15) 0.52020(10) 0.21105(9) 0.0273(3) Uani 1 1 d . . . S4 S -0.07737(16) 0.31657(10) 0.39678(10) 0.0306(3) Uani 1 1 d . . . C5 C -0.0707(7) 0.3238(4) 0.5229(4) 0.0344(11) Uani 1 1 d . . . H5A H -0.1170 0.3958 0.5219 0.041 Uiso 1 1 calc R . . H5B H -0.1484 0.2597 0.5874 0.041 Uiso 1 1 calc R . . C6 C 0.1198(7) 0.3182(4) 0.5317(4) 0.0337(11) Uani 1 1 d . . . H6A H 0.1278 0.3303 0.5956 0.040 Uiso 1 1 calc R . . H6B H 0.1625 0.2429 0.5413 0.040 Uiso 1 1 calc R . . C7 C 0.4152(7) 0.4126(5) 0.4320(4) 0.0347(11) Uani 1 1 d . . . H7A H 0.4725 0.3452 0.4276 0.042 Uiso 1 1 calc R . . H7B H 0.4216 0.4131 0.5016 0.042 Uiso 1 1 calc R . . C8 C 0.5102(6) 0.5185(4) 0.3361(4) 0.0302(10) Uani 1 1 d . . . H8A H 0.6405 0.5210 0.3318 0.036 Uiso 1 1 calc R . . H8B H 0.4610 0.5860 0.3447 0.036 Uiso 1 1 calc R . . O12 O 0.2289(4) 0.4081(3) 0.4293(2) 0.0259(7) Uani 1 1 d . . . C21 C 0.0560(6) 0.5679(4) 0.0893(3) 0.0257(10) Uani 1 1 d . . . C22 C 0.2417(6) 0.5535(4) 0.0629(4) 0.0294(10) Uani 1 1 d . . . H22 H 0.3365 0.6127 0.0267 0.035 Uiso 1 1 calc R . . C23 C 0.2629(7) 0.4339(5) 0.1003(4) 0.0330(11) Uani 1 1 d . . . H23 H 0.3740 0.4008 0.0898 0.040 Uiso 1 1 calc R . . C24 C 0.0963(7) 0.3758(4) 0.1534(4) 0.0295(10) Uani 1 1 d . . . H24 H 0.0713 0.2955 0.1863 0.035 Uiso 1 1 calc R . . C25 C -0.0345(6) 0.4581(4) 0.1504(4) 0.0254(9) Uani 1 1 d . . . H25 H -0.1605 0.4413 0.1839 0.030 Uiso 1 1 calc R . . C26 C -0.0280(7) 0.6785(4) 0.0620(4) 0.0358(11) Uani 1 1 d . . . H26A H -0.1247 0.6796 0.0277 0.054 Uiso 1 1 calc R . . H26B H 0.0638 0.7413 0.0108 0.054 Uiso 1 1 calc R . . H26C H -0.0782 0.6873 0.1297 0.054 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 0.0191(2) 0.0177(2) 0.0208(2) -0.00907(15) -0.00731(15) 0.00135(15) O1 0.044(2) 0.0319(19) 0.0273(17) -0.0135(14) -0.0071(15) -0.0107(15) S1 0.0297(6) 0.0333(7) 0.0519(8) -0.0274(6) -0.0179(5) 0.0127(5) O11 0.0336(17) 0.0226(16) 0.0299(17) -0.0151(13) -0.0128(14) 0.0014(13) S2 0.0242(6) 0.0419(7) 0.0480(7) -0.0293(6) -0.0189(5) 0.0118(5) C1 0.038(3) 0.029(3) 0.040(3) -0.021(2) -0.001(2) 0.005(2) C2 0.046(3) 0.028(3) 0.033(3) -0.021(2) -0.011(2) 0.003(2) C3 0.037(3) 0.030(3) 0.033(3) -0.012(2) -0.019(2) -0.004(2) C4 0.031(3) 0.040(3) 0.030(2) -0.011(2) -0.019(2) 0.002(2) C11 0.027(2) 0.026(2) 0.025(2) -0.0147(18) -0.0129(18) 0.0006(18) C12 0.029(2) 0.029(2) 0.029(2) -0.019(2) -0.0141(19) 0.0065(19) C13 0.025(2) 0.036(3) 0.023(2) -0.0152(19) -0.0072(18) -0.0014(19) C14 0.036(3) 0.022(2) 0.023(2) -0.0085(18) -0.0127(19) -0.0010(19) C15 0.027(2) 0.030(2) 0.023(2) -0.0138(19) -0.0130(18) 0.0050(19) C16 0.040(3) 0.025(2) 0.040(3) -0.013(2) -0.014(2) -0.006(2) Nb2 0.0179(2) 0.0183(2) 0.0190(2) -0.00937(15) -0.00679(14) 0.00229(14) O2 0.0321(17) 0.0246(16) 0.0248(15) -0.0129(13) -0.0123(13) 0.0040(13) S3 0.0203(5) 0.0332(6) 0.0319(6) -0.0163(5) -0.0091(4) 0.0023(4) S4 0.0322(6) 0.0292(6) 0.0270(6) -0.0095(5) -0.0059(5) -0.0089(5) C5 0.041(3) 0.031(3) 0.027(2) -0.013(2) 0.000(2) -0.008(2) C6 0.050(3) 0.026(2) 0.023(2) -0.0058(19) -0.015(2) 0.000(2) C7 0.033(3) 0.040(3) 0.041(3) -0.018(2) -0.025(2) 0.008(2) C8 0.027(2) 0.034(3) 0.039(3) -0.020(2) -0.018(2) 0.002(2) O12 0.0292(16) 0.0250(16) 0.0232(15) -0.0073(13) -0.0123(13) 0.0009(13) C21 0.030(2) 0.030(3) 0.021(2) -0.0121(19) -0.0120(18) 0.0051(19) C22 0.028(2) 0.040(3) 0.024(2) -0.016(2) -0.0084(19) 0.000(2) C23 0.032(3) 0.051(3) 0.027(2) -0.027(2) -0.011(2) 0.016(2) C24 0.043(3) 0.030(3) 0.031(2) -0.022(2) -0.019(2) 0.008(2) C25 0.026(2) 0.028(2) 0.029(2) -0.0147(19) -0.0127(18) 0.0012(18) C26 0.047(3) 0.029(3) 0.039(3) -0.015(2) -0.024(2) 0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 O1 1.734(3) . y Nb1 O11 2.351(3) . y Nb1 C15 2.431(4) . ? Nb1 C12 2.439(4) . ? Nb1 C11 2.468(4) . ? Nb1 S1 2.4732(13) . y Nb1 S2 2.4761(13) . y Nb1 C14 2.497(4) . ? Nb1 C13 2.507(4) . ? S1 C1 1.813(5) . y O11 C3 1.441(6) . y O11 C2 1.455(6) . y S2 C4 1.814(5) . y C1 C2 1.494(7) . y C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.500(7) . y C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C11 C15 1.403(6) . ? C11 C12 1.417(6) . ? C11 C16 1.495(6) . ? C12 C13 1.444(7) . ? C12 H12 0.9500 . ? C13 C14 1.372(7) . ? C13 H13 0.9500 . ? C14 C15 1.434(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? Nb2 O2 1.735(3) . y Nb2 O12 2.342(3) . y Nb2 C22 2.434(4) . ? Nb2 C25 2.447(4) . ? Nb2 S4 2.4651(13) . y Nb2 C21 2.473(4) . ? Nb2 S3 2.4743(13) . y Nb2 C23 2.507(4) . ? Nb2 C24 2.517(4) . ? S3 C8 1.819(5) . y S4 C5 1.820(5) . y C5 C6 1.499(7) . y C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O12 1.460(5) . y C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O12 1.448(5) . y C7 C8 1.488(7) . y C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C21 C22 1.407(7) . ? C21 C25 1.409(7) . ? C21 C26 1.495(7) . ? C22 C23 1.437(7) . ? C22 H22 0.9500 . ? C23 C24 1.368(7) . ? C23 H23 0.9500 . ? C24 C25 1.440(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 O1 Nb1 O11 90.65(13) . . y O1 Nb1 C15 101.60(16) . . ? O11 Nb1 C15 148.91(13) . . ? O1 Nb1 C12 99.21(16) . . ? O11 Nb1 C12 150.69(13) . . ? C15 Nb1 C12 55.52(15) . . ? O1 Nb1 C11 82.40(15) . . ? O11 Nb1 C11 172.91(13) . . ? C15 Nb1 C11 33.29(15) . . ? C12 Nb1 C11 33.55(15) . . ? O1 Nb1 S1 104.45(13) . . y O11 Nb1 S1 74.38(8) . . y C15 Nb1 S1 74.92(11) . . ? C12 Nb1 S1 128.34(11) . . ? C11 Nb1 S1 105.91(11) . . ? O1 Nb1 S2 105.65(13) . . y O11 Nb1 S2 74.03(8) . . y C15 Nb1 S2 127.94(11) . . ? C12 Nb1 S2 76.74(11) . . ? C11 Nb1 S2 109.15(11) . . ? S1 Nb1 S2 136.06(5) . . y O1 Nb1 C14 134.79(16) . . ? O11 Nb1 C14 130.82(13) . . ? C15 Nb1 C14 33.82(15) . . ? C12 Nb1 C14 55.02(15) . . ? C11 Nb1 C14 55.33(15) . . ? S1 Nb1 C14 76.21(11) . . ? S2 Nb1 C14 103.12(11) . . ? O1 Nb1 C13 132.91(16) . . ? O11 Nb1 C13 131.63(13) . . ? C15 Nb1 C13 54.78(15) . . ? C12 Nb1 C13 33.91(15) . . ? C11 Nb1 C13 55.34(15) . . ? S1 Nb1 C13 106.28(11) . . ? S2 Nb1 C13 74.35(11) . . ? C14 Nb1 C13 31.83(15) . . ? C1 S1 Nb1 99.38(17) . . y C3 O11 C2 110.6(3) . . y C3 O11 Nb1 122.6(3) . . y C2 O11 Nb1 122.2(3) . . y C4 S2 Nb1 100.34(17) . . y C2 C1 S1 110.1(3) . . ? C2 C1 H1A 109.6 . . ? S1 C1 H1A 109.6 . . ? C2 C1 H1B 109.6 . . ? S1 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? O11 C2 C1 107.2(4) . . ? O11 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? O11 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? O11 C3 C4 107.5(4) . . ? O11 C3 H3A 110.2 . . ? C4 C3 H3A 110.2 . . ? O11 C3 H3B 110.2 . . ? C4 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? C3 C4 S2 109.4(3) . . ? C3 C4 H4A 109.8 . . ? S2 C4 H4A 109.8 . . ? C3 C4 H4B 109.8 . . ? S2 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? C15 C11 C12 107.1(4) . . ? C15 C11 C16 126.5(4) . . ? C12 C11 C16 126.3(4) . . ? C15 C11 Nb1 71.9(3) . . ? C12 C11 Nb1 72.1(2) . . ? C16 C11 Nb1 119.5(3) . . ? C11 C12 C13 107.7(4) . . ? C11 C12 Nb1 74.3(3) . . ? C13 C12 Nb1 75.6(3) . . ? C11 C12 H12 126.1 . . ? C13 C12 H12 126.1 . . ? Nb1 C12 H12 116.1 . . ? C14 C13 C12 108.2(4) . . ? C14 C13 Nb1 73.7(3) . . ? C12 C13 Nb1 70.5(2) . . ? C14 C13 H13 125.9 . . ? C12 C13 H13 125.9 . . ? Nb1 C13 H13 121.6 . . ? C13 C14 C15 108.1(4) . . ? C13 C14 Nb1 74.5(3) . . ? C15 C14 Nb1 70.6(2) . . ? C13 C14 H14 125.9 . . ? C15 C14 H14 125.9 . . ? Nb1 C14 H14 120.7 . . ? C11 C15 C14 108.6(4) . . ? C11 C15 Nb1 74.8(2) . . ? C14 C15 Nb1 75.6(3) . . ? C11 C15 H15 125.7 . . ? C14 C15 H15 125.7 . . ? Nb1 C15 H15 115.9 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O2 Nb2 O12 90.82(12) . . y O2 Nb2 C22 101.89(15) . . ? O12 Nb2 C22 148.50(14) . . ? O2 Nb2 C25 99.90(15) . . ? O12 Nb2 C25 150.84(13) . . ? C22 Nb2 C25 55.20(16) . . ? O2 Nb2 S4 102.77(11) . . y O12 Nb2 S4 74.34(8) . . y C22 Nb2 S4 128.90(12) . . ? C25 Nb2 S4 76.85(11) . . ? O2 Nb2 C21 82.91(15) . . ? O12 Nb2 C21 173.56(13) . . ? C22 Nb2 C21 33.32(15) . . ? C25 Nb2 C21 33.27(15) . . ? S4 Nb2 C21 108.41(11) . . ? O2 Nb2 S3 104.62(11) . . y O12 Nb2 S3 74.20(8) . . y C22 Nb2 S3 74.73(11) . . ? C25 Nb2 S3 127.68(11) . . ? S4 Nb2 S3 138.13(4) . . y C21 Nb2 S3 105.89(11) . . ? O2 Nb2 C23 135.02(15) . . ? O12 Nb2 C23 130.38(14) . . ? C22 Nb2 C23 33.76(17) . . ? C25 Nb2 C23 54.44(16) . . ? S4 Nb2 C23 105.15(13) . . ? C21 Nb2 C23 55.10(15) . . ? S3 Nb2 C23 76.02(12) . . ? O2 Nb2 C24 133.39(15) . . ? O12 Nb2 C24 131.16(13) . . ? C22 Nb2 C24 54.72(17) . . ? C25 Nb2 C24 33.69(15) . . ? S4 Nb2 C24 76.01(12) . . ? C21 Nb2 C24 55.20(16) . . ? S3 Nb2 C24 105.77(12) . . ? C23 Nb2 C24 31.59(17) . . ? C8 S3 Nb2 101.46(16) . . y C5 S4 Nb2 99.13(16) . . y C6 C5 S4 109.4(3) . . ? C6 C5 H5A 109.8 . . ? S4 C5 H5A 109.8 . . ? C6 C5 H5B 109.8 . . ? S4 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? O12 C6 C5 106.7(4) . . ? O12 C6 H6A 110.4 . . ? C5 C6 H6A 110.4 . . ? O12 C6 H6B 110.4 . . ? C5 C6 H6B 110.4 . . ? H6A C6 H6B 108.6 . . ? O12 C7 C8 107.9(4) . . ? O12 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? O12 C7 H7B 110.1 . . ? C8 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? C7 C8 S3 108.7(3) . . ? C7 C8 H8A 109.9 . . ? S3 C8 H8A 109.9 . . ? C7 C8 H8B 109.9 . . ? S3 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C7 O12 C6 110.8(3) . . y C7 O12 Nb2 121.9(3) . . y C6 O12 Nb2 122.4(3) . . y C22 C21 C25 106.8(4) . . ? C22 C21 C26 126.4(4) . . ? C25 C21 C26 126.7(4) . . ? C22 C21 Nb2 71.8(3) . . ? C25 C21 Nb2 72.3(2) . . ? C26 C21 Nb2 119.1(3) . . ? C21 C22 C23 108.2(4) . . ? C21 C22 Nb2 74.8(3) . . ? C23 C22 Nb2 75.9(3) . . ? C21 C22 H22 125.9 . . ? C23 C22 H22 125.9 . . ? Nb2 C22 H22 115.5 . . ? C24 C23 C22 108.6(4) . . ? C24 C23 Nb2 74.6(3) . . ? C22 C23 Nb2 70.3(3) . . ? C24 C23 H23 125.7 . . ? C22 C23 H23 125.7 . . ? Nb2 C23 H23 121.0 . . ? C23 C24 C25 107.6(4) . . ? C23 C24 Nb2 73.8(3) . . ? C25 C24 Nb2 70.5(2) . . ? C23 C24 H24 126.2 . . ? C25 C24 H24 126.2 . . ? Nb2 C24 H24 121.3 . . ? C21 C25 C24 108.5(4) . . ? C21 C25 Nb2 74.4(2) . . ? C24 C25 Nb2 75.9(2) . . ? C21 C25 H25 125.7 . . ? C24 C25 H25 125.7 . . ? Nb2 C25 H25 116.1 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 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 O1 Nb1 S1 C1 -60.2(2) . . . . ? O11 Nb1 S1 C1 26.40(19) . . . . ? C15 Nb1 S1 C1 -158.5(2) . . . . ? C12 Nb1 S1 C1 -174.7(2) . . . . ? C11 Nb1 S1 C1 -146.2(2) . . . . ? S2 Nb1 S1 C1 71.82(19) . . . . ? C14 Nb1 S1 C1 166.5(2) . . . . ? C13 Nb1 S1 C1 156.0(2) . . . . ? O1 Nb1 O11 C3 -104.9(3) . . . . ? C15 Nb1 O11 C3 141.0(3) . . . . ? C12 Nb1 O11 C3 5.4(5) . . . . ? S1 Nb1 O11 C3 150.3(3) . . . . ? S2 Nb1 O11 C3 1.2(3) . . . . ? C14 Nb1 O11 C3 94.9(3) . . . . ? C13 Nb1 O11 C3 52.2(4) . . . . ? O1 Nb1 O11 C2 101.4(3) . . . . ? C15 Nb1 O11 C2 -12.7(5) . . . . ? C12 Nb1 O11 C2 -148.3(3) . . . . ? S1 Nb1 O11 C2 -3.5(3) . . . . ? S2 Nb1 O11 C2 -152.5(3) . . . . ? C14 Nb1 O11 C2 -58.8(4) . . . . ? C13 Nb1 O11 C2 -101.6(3) . . . . ? O1 Nb1 S2 C4 61.1(2) . . . . ? O11 Nb1 S2 C4 -25.03(19) . . . . ? C15 Nb1 S2 C4 180.0(2) . . . . ? C12 Nb1 S2 C4 157.1(2) . . . . ? C11 Nb1 S2 C4 148.3(2) . . . . ? S1 Nb1 S2 C4 -70.55(19) . . . . ? C14 Nb1 S2 C4 -154.2(2) . . . . ? C13 Nb1 S2 C4 -168.0(2) . . . . ? Nb1 S1 C1 C2 -53.3(4) . . . . ? C3 O11 C2 C1 175.9(4) . . . . ? Nb1 O11 C2 C1 -27.5(5) . . . . ? S1 C1 C2 O11 53.6(5) . . . . ? C2 O11 C3 C4 -173.9(4) . . . . ? Nb1 O11 C3 C4 29.6(5) . . . . ? O11 C3 C4 S2 -53.4(4) . . . . ? Nb1 S2 C4 C3 51.6(4) . . . . ? O1 Nb1 C11 C15 -125.0(3) . . . . ? C12 Nb1 C11 C15 115.5(4) . . . . ? S1 Nb1 C11 C15 -22.0(3) . . . . ? S2 Nb1 C11 C15 131.1(2) . . . . ? C14 Nb1 C11 C15 38.1(3) . . . . ? C13 Nb1 C11 C15 77.0(3) . . . . ? O1 Nb1 C11 C12 119.6(3) . . . . ? C15 Nb1 C11 C12 -115.5(4) . . . . ? S1 Nb1 C11 C12 -137.5(2) . . . . ? S2 Nb1 C11 C12 15.6(3) . . . . ? C14 Nb1 C11 C12 -77.4(3) . . . . ? C13 Nb1 C11 C12 -38.5(3) . . . . ? O1 Nb1 C11 C16 -2.6(4) . . . . ? C15 Nb1 C11 C16 122.3(5) . . . . ? C12 Nb1 C11 C16 -122.2(5) . . . . ? S1 Nb1 C11 C16 100.3(3) . . . . ? S2 Nb1 C11 C16 -106.6(3) . . . . ? C14 Nb1 C11 C16 160.4(4) . . . . ? C13 Nb1 C11 C16 -160.7(4) . . . . ? C15 C11 C12 C13 5.0(5) . . . . ? C16 C11 C12 C13 -177.3(4) . . . . ? Nb1 C11 C12 C13 68.8(3) . . . . ? C15 C11 C12 Nb1 -63.9(3) . . . . ? C16 C11 C12 Nb1 113.9(4) . . . . ? O1 Nb1 C12 C11 -60.9(3) . . . . ? O11 Nb1 C12 C11 -169.1(2) . . . . ? C15 Nb1 C12 C11 36.9(3) . . . . ? S1 Nb1 C12 C11 55.9(3) . . . . ? S2 Nb1 C12 C11 -164.9(3) . . . . ? C14 Nb1 C12 C11 78.4(3) . . . . ? C13 Nb1 C12 C11 113.5(4) . . . . ? O1 Nb1 C12 C13 -174.4(3) . . . . ? O11 Nb1 C12 C13 77.4(4) . . . . ? C15 Nb1 C12 C13 -76.6(3) . . . . ? C11 Nb1 C12 C13 -113.5(4) . . . . ? S1 Nb1 C12 C13 -57.6(3) . . . . ? S2 Nb1 C12 C13 81.6(2) . . . . ? C14 Nb1 C12 C13 -35.1(3) . . . . ? C11 C12 C13 C14 -3.4(5) . . . . ? Nb1 C12 C13 C14 64.5(3) . . . . ? C11 C12 C13 Nb1 -68.0(3) . . . . ? O1 Nb1 C13 C14 -109.0(3) . . . . ? O11 Nb1 C13 C14 103.1(3) . . . . ? C15 Nb1 C13 C14 -37.7(3) . . . . ? C12 Nb1 C13 C14 -116.6(4) . . . . ? C11 Nb1 C13 C14 -78.6(3) . . . . ? S1 Nb1 C13 C14 19.7(3) . . . . ? S2 Nb1 C13 C14 153.9(3) . . . . ? O1 Nb1 C13 C12 7.6(4) . . . . ? O11 Nb1 C13 C12 -140.3(2) . . . . ? C15 Nb1 C13 C12 78.9(3) . . . . ? C11 Nb1 C13 C12 38.0(3) . . . . ? S1 Nb1 C13 C12 136.4(2) . . . . ? S2 Nb1 C13 C12 -89.4(2) . . . . ? C14 Nb1 C13 C12 116.6(4) . . . . ? C12 C13 C14 C15 0.5(5) . . . . ? Nb1 C13 C14 C15 63.0(3) . . . . ? C12 C13 C14 Nb1 -62.5(3) . . . . ? O1 Nb1 C14 C13 102.7(3) . . . . ? O11 Nb1 C14 C13 -105.8(3) . . . . ? C15 Nb1 C14 C13 116.1(4) . . . . ? C12 Nb1 C14 C13 37.5(3) . . . . ? C11 Nb1 C14 C13 78.6(3) . . . . ? S1 Nb1 C14 C13 -160.5(3) . . . . ? S2 Nb1 C14 C13 -25.7(3) . . . . ? O1 Nb1 C14 C15 -13.4(4) . . . . ? O11 Nb1 C14 C15 138.1(2) . . . . ? C12 Nb1 C14 C15 -78.6(3) . . . . ? C11 Nb1 C14 C15 -37.5(3) . . . . ? S1 Nb1 C14 C15 83.4(3) . . . . ? S2 Nb1 C14 C15 -141.8(2) . . . . ? C13 Nb1 C14 C15 -116.1(4) . . . . ? C12 C11 C15 C14 -4.7(5) . . . . ? C16 C11 C15 C14 177.6(4) . . . . ? Nb1 C11 C15 C14 -68.7(3) . . . . ? C12 C11 C15 Nb1 64.0(3) . . . . ? C16 C11 C15 Nb1 -113.7(4) . . . . ? C13 C14 C15 C11 2.6(5) . . . . ? Nb1 C14 C15 C11 68.2(3) . . . . ? C13 C14 C15 Nb1 -65.6(3) . . . . ? O1 Nb1 C15 C11 56.0(3) . . . . ? O11 Nb1 C15 C11 167.3(2) . . . . ? C12 Nb1 C15 C11 -37.2(3) . . . . ? S1 Nb1 C15 C11 158.1(3) . . . . ? S2 Nb1 C15 C11 -64.6(3) . . . . ? C14 Nb1 C15 C11 -114.3(4) . . . . ? C13 Nb1 C15 C11 -78.9(3) . . . . ? O1 Nb1 C15 C14 170.3(3) . . . . ? O11 Nb1 C15 C14 -78.4(4) . . . . ? C12 Nb1 C15 C14 77.0(3) . . . . ? C11 Nb1 C15 C14 114.3(4) . . . . ? S1 Nb1 C15 C14 -87.6(3) . . . . ? S2 Nb1 C15 C14 49.7(3) . . . . ? C13 Nb1 C15 C14 35.4(3) . . . . ? O2 Nb2 S3 C8 64.8(2) . . . . ? O12 Nb2 S3 C8 -21.87(18) . . . . ? C22 Nb2 S3 C8 163.4(2) . . . . ? C25 Nb2 S3 C8 180.0(2) . . . . ? S4 Nb2 S3 C8 -64.50(18) . . . . ? C21 Nb2 S3 C8 151.4(2) . . . . ? C23 Nb2 S3 C8 -161.7(2) . . . . ? C24 Nb2 S3 C8 -151.0(2) . . . . ? O2 Nb2 S4 C5 -59.6(2) . . . . ? O12 Nb2 S4 C5 27.6(2) . . . . ? C22 Nb2 S4 C5 -176.6(2) . . . . ? C25 Nb2 S4 C5 -157.0(2) . . . . ? C21 Nb2 S4 C5 -146.3(2) . . . . ? S3 Nb2 S4 C5 70.22(19) . . . . ? C23 Nb2 S4 C5 156.0(2) . . . . ? C24 Nb2 S4 C5 168.4(2) . . . . ? Nb2 S4 C5 C6 -54.7(3) . . . . ? S4 C5 C6 O12 54.0(4) . . . . ? O12 C7 C8 S3 -54.7(5) . . . . ? Nb2 S3 C8 C7 49.1(3) . . . . ? C8 C7 O12 C6 -169.3(4) . . . . ? C8 C7 O12 Nb2 35.1(5) . . . . ? C5 C6 O12 C7 177.5(4) . . . . ? C5 C6 O12 Nb2 -27.0(5) . . . . ? O2 Nb2 O12 C7 -108.8(3) . . . . ? C22 Nb2 O12 C7 5.9(5) . . . . ? C25 Nb2 O12 C7 139.0(4) . . . . ? S4 Nb2 O12 C7 148.2(3) . . . . ? S3 Nb2 O12 C7 -3.8(3) . . . . ? C23 Nb2 O12 C7 51.4(4) . . . . ? C24 Nb2 O12 C7 93.5(4) . . . . ? O2 Nb2 O12 C6 98.4(3) . . . . ? C25 Nb2 O12 C6 -13.8(5) . . . . ? S4 Nb2 O12 C6 -4.6(3) . . . . ? S3 Nb2 O12 C6 -156.6(3) . . . . ? C23 Nb2 O12 C6 -101.4(4) . . . . ? C24 Nb2 O12 C6 -59.3(4) . . . . ? O2 Nb2 C21 C22 124.5(3) . . . . ? C25 Nb2 C21 C22 -115.1(4) . . . . ? S4 Nb2 C21 C22 -134.3(3) . . . . ? S3 Nb2 C21 C22 21.3(3) . . . . ? C23 Nb2 C21 C22 -38.4(3) . . . . ? C24 Nb2 C21 C22 -77.1(3) . . . . ? O2 Nb2 C21 C25 -120.3(3) . . . . ? C22 Nb2 C21 C25 115.1(4) . . . . ? S4 Nb2 C21 C25 -19.2(3) . . . . ? S3 Nb2 C21 C25 136.4(2) . . . . ? C23 Nb2 C21 C25 76.8(3) . . . . ? C24 Nb2 C21 C25 38.0(3) . . . . ? O2 Nb2 C21 C26 2.4(4) . . . . ? C22 Nb2 C21 C26 -122.2(5) . . . . ? C25 Nb2 C21 C26 122.7(5) . . . . ? S4 Nb2 C21 C26 103.5(4) . . . . ? S3 Nb2 C21 C26 -100.9(4) . . . . ? C23 Nb2 C21 C26 -160.5(4) . . . . ? C24 Nb2 C21 C26 160.7(4) . . . . ? C25 C21 C22 C23 4.9(5) . . . . ? C26 C21 C22 C23 -177.6(4) . . . . ? Nb2 C21 C22 C23 69.2(3) . . . . ? C25 C21 C22 Nb2 -64.3(3) . . . . ? C26 C21 C22 Nb2 113.2(5) . . . . ? O2 Nb2 C22 C21 -56.7(3) . . . . ? C25 Nb2 C22 C21 37.2(3) . . . . ? S4 Nb2 C22 C21 60.7(3) . . . . ? S3 Nb2 C22 C21 -158.8(3) . . . . ? C23 Nb2 C22 C21 113.7(4) . . . . ? C24 Nb2 C22 C21 78.7(3) . . . . ? O2 Nb2 C22 C23 -170.3(3) . . . . ? O12 Nb2 C22 C23 77.9(4) . . . . ? C25 Nb2 C22 C23 -76.4(3) . . . . ? S4 Nb2 C22 C23 -52.9(3) . . . . ? C21 Nb2 C22 C23 -113.7(4) . . . . ? S3 Nb2 C22 C23 87.6(3) . . . . ? C24 Nb2 C22 C23 -35.0(3) . . . . ? C21 C22 C23 C24 -3.2(5) . . . . ? Nb2 C22 C23 C24 65.3(3) . . . . ? C21 C22 C23 Nb2 -68.5(3) . . . . ? O2 Nb2 C23 C24 -103.2(3) . . . . ? O12 Nb2 C23 C24 105.4(3) . . . . ? C22 Nb2 C23 C24 -116.7(4) . . . . ? C25 Nb2 C23 C24 -37.8(3) . . . . ? S4 Nb2 C23 C24 23.3(3) . . . . ? C21 Nb2 C23 C24 -78.8(3) . . . . ? S3 Nb2 C23 C24 160.0(3) . . . . ? O2 Nb2 C23 C22 13.5(4) . . . . ? O12 Nb2 C23 C22 -137.9(3) . . . . ? C25 Nb2 C23 C22 78.9(3) . . . . ? S4 Nb2 C23 C22 140.0(3) . . . . ? C21 Nb2 C23 C22 37.8(3) . . . . ? S3 Nb2 C23 C22 -83.3(3) . . . . ? C24 Nb2 C23 C22 116.7(4) . . . . ? C22 C23 C24 C25 0.2(5) . . . . ? Nb2 C23 C24 C25 62.7(3) . . . . ? C22 C23 C24 Nb2 -62.6(3) . . . . ? O2 Nb2 C24 C23 108.7(3) . . . . ? O12 Nb2 C24 C23 -102.8(3) . . . . ? C22 Nb2 C24 C23 37.5(3) . . . . ? C25 Nb2 C24 C23 116.0(4) . . . . ? S4 Nb2 C24 C23 -156.8(3) . . . . ? C21 Nb2 C24 C23 78.5(3) . . . . ? S3 Nb2 C24 C23 -20.2(3) . . . . ? O2 Nb2 C24 C25 -7.3(4) . . . . ? O12 Nb2 C24 C25 141.2(2) . . . . ? C22 Nb2 C24 C25 -78.5(3) . . . . ? S4 Nb2 C24 C25 87.2(3) . . . . ? C21 Nb2 C24 C25 -37.5(3) . . . . ? S3 Nb2 C24 C25 -136.2(3) . . . . ? C23 Nb2 C24 C25 -116.0(4) . . . . ? C22 C21 C25 C24 -4.8(5) . . . . ? C26 C21 C25 C24 177.7(4) . . . . ? Nb2 C21 C25 C24 -68.8(3) . . . . ? C22 C21 C25 Nb2 64.0(3) . . . . ? C26 C21 C25 Nb2 -113.5(5) . . . . ? C23 C24 C25 C21 2.9(5) . . . . ? Nb2 C24 C25 C21 67.8(3) . . . . ? C23 C24 C25 Nb2 -64.9(3) . . . . ? O2 Nb2 C25 C21 60.4(3) . . . . ? O12 Nb2 C25 C21 170.4(2) . . . . ? C22 Nb2 C25 C21 -37.3(3) . . . . ? S4 Nb2 C25 C21 161.3(3) . . . . ? S3 Nb2 C25 C21 -56.9(3) . . . . ? C23 Nb2 C25 C21 -78.9(3) . . . . ? C24 Nb2 C25 C21 -114.3(4) . . . . ? O2 Nb2 C25 C24 174.6(3) . . . . ? O12 Nb2 C25 C24 -75.3(4) . . . . ? C22 Nb2 C25 C24 77.0(3) . . . . ? S4 Nb2 C25 C24 -84.4(3) . . . . ? C21 Nb2 C25 C24 114.3(4) . . . . ? S3 Nb2 C25 C24 57.4(3) . . . . ? C23 Nb2 C25 C24 35.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.885 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.116