# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Guido Pampaloni' _publ_contact_author_email PAMPA@DCCI.UNIPI.IT _publ_section_title ; ations of Oxygen-containing Molecules via C-O Bonds Cleavage Promoted by Coordination to Niobium and Tantalum Pentahalides ; loop_ _publ_author_name 'Guido Pampaloni' 'Fabio Marchetti' 'Stefano Zacchini' # Attachment 'Compound_3b.CIF' data_pca21 _database_code_depnum_ccdc_archive 'CCDC 723065' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 Br8 Nb2 O4' _chemical_formula_weight 945.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 13.6421(18) _cell_length_b 9.6914(13) _cell_length_c 13.9238(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1840.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3479 _cell_measurement_theta_min 2.578 _cell_measurement_theta_max 28.138 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 18.609 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1667 _exptl_absorpt_correction_T_max 0.2577 _exptl_absorpt_process_details 'SADABS (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11425 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3580 _reflns_number_gt 3184 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1043P)^2^+26.5580P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(2) _refine_ls_number_reflns 3580 _refine_ls_number_parameters 164 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1640 _refine_ls_wR_factor_gt 0.1569 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.134 _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 Br1 Br 1.12179(14) 0.8388(2) 0.86634(14) 0.0263(4) Uani 1 1 d . . . Br2 Br 0.91471(15) 1.03905(19) 0.91199(13) 0.0249(4) Uani 1 1 d . . . Br3 Br 0.81300(15) 0.9215(2) 0.69488(17) 0.0316(5) Uani 1 1 d U . . Br4 Br 1.02782(17) 0.7354(2) 0.65345(18) 0.0381(5) Uani 1 1 d U . . Br5 Br 1.04629(15) 1.0929(2) 0.68955(16) 0.0293(5) Uani 1 1 d U . . Br6 Br 0.96301(15) 0.4087(2) 0.81834(17) 0.0296(5) Uani 1 1 d U . . Br7 Br 0.94512(16) 0.6057(2) 1.04079(15) 0.0323(5) Uani 1 1 d U . . Br8 Br 0.72252(14) 0.5414(2) 0.77502(16) 0.0323(5) Uani 1 1 d U . . Nb1 Nb 0.97496(10) 0.90190(14) 0.77307(10) 0.0079(3) Uani 1 1 d U . . Nb2 Nb 0.85824(10) 0.57770(13) 0.88912(10) 0.0077(3) Uani 1 1 d U . . C1 C 0.6904(13) 0.8082(16) 0.9326(12) 0.015(3) Uani 1 1 d U . . H1A H 0.7358 0.8585 0.8932 0.022 Uiso 1 1 calc R . . H1B H 0.6704 0.8648 0.9857 0.022 Uiso 1 1 calc R . . H1C H 0.6340 0.7833 0.8951 0.022 Uiso 1 1 calc R . . C2 C 0.6714(12) 0.6060(17) 1.0280(12) 0.011(2) Uani 1 1 d U . . H2A H 0.6061 0.6046 1.0004 0.013 Uiso 1 1 calc R . . H2B H 0.6676 0.6462 1.0917 0.013 Uiso 1 1 calc R . . C3 C 0.7128(12) 0.4601(17) 1.0335(11) 0.012(2) Uani 1 1 d U . . C4 C 0.7000(11) 0.2464(16) 1.1110(12) 0.012(3) Uani 1 1 d U . . H4A H 0.6617 0.2047 1.1611 0.017 Uiso 1 1 calc R . . H4B H 0.7680 0.2450 1.1288 0.017 Uiso 1 1 calc R . . H4C H 0.6911 0.1957 1.0524 0.017 Uiso 1 1 calc R . . O1 O 0.9024(8) 0.7308(11) 0.8390(8) 0.0138(17) Uani 1 1 d U . . O2 O 0.7370(8) 0.6854(11) 0.9682(8) 0.0126(17) Uani 1 1 d U . . O3 O 0.7767(9) 0.4247(11) 0.9772(9) 0.0187(18) Uani 1 1 d U . . O4 O 0.6683(8) 0.3887(11) 1.0972(8) 0.012(2) Uani 1 1 d U . . 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 Br1 0.0239(10) 0.0257(9) 0.0294(10) 0.0051(8) -0.0121(8) -0.0030(7) Br2 0.0309(10) 0.0206(9) 0.0233(9) -0.0085(7) 0.0062(8) -0.0057(8) Br3 0.0213(8) 0.0368(11) 0.0368(11) 0.0055(9) -0.0062(8) 0.0000(7) Br4 0.0363(11) 0.0353(10) 0.0426(12) -0.0168(9) 0.0048(9) 0.0011(8) Br5 0.0287(10) 0.0245(9) 0.0346(11) 0.0119(7) 0.0020(9) -0.0058(7) Br6 0.0257(9) 0.0230(10) 0.0400(11) -0.0046(7) 0.0067(8) 0.0092(7) Br7 0.0338(11) 0.0353(12) 0.0277(9) -0.0003(8) -0.0079(8) 0.0012(9) Br8 0.0209(8) 0.0423(12) 0.0338(10) -0.0087(9) -0.0032(7) -0.0015(8) Nb1 0.0073(6) 0.0058(6) 0.0104(6) 0.0015(5) -0.0006(5) -0.0013(5) Nb2 0.0058(6) 0.0036(6) 0.0136(6) 0.0029(5) 0.0049(5) 0.0001(5) C1 0.016(5) 0.009(4) 0.020(5) 0.000(4) 0.003(4) 0.005(3) C2 0.012(4) 0.013(3) 0.009(4) 0.002(3) 0.004(3) 0.003(3) C3 0.013(4) 0.011(3) 0.011(4) 0.003(3) 0.003(3) 0.000(3) C4 0.010(5) 0.010(4) 0.015(5) 0.002(4) 0.000(4) -0.004(4) O1 0.008(5) 0.012(3) 0.022(4) -0.002(3) -0.001(3) -0.003(3) O2 0.011(3) 0.010(3) 0.017(4) 0.003(3) 0.004(3) 0.001(3) O3 0.022(4) 0.008(3) 0.026(4) -0.002(3) 0.010(3) 0.000(3) O4 0.004(5) 0.014(4) 0.017(5) 0.004(4) 0.002(4) 0.000(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 Br1 Nb1 2.464(2) . ? Br2 Nb1 2.487(2) . ? Br3 Nb1 2.470(2) . ? Br4 Nb1 2.429(3) . ? Br5 Nb1 2.392(2) . ? Br6 Nb2 2.387(2) . ? Br7 Nb2 2.437(3) . ? Br8 Nb2 2.465(2) . ? Nb1 O1 2.138(11) . ? Nb2 O1 1.747(11) . ? Nb2 O3 2.222(12) . ? Nb2 O2 2.244(11) . ? C1 O2 1.437(19) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O2 1.444(19) . ? C2 C3 1.52(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 O3 1.22(2) . ? C3 O4 1.28(2) . ? C4 O4 1.458(19) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 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 O1 Nb1 Br5 175.4(3) . . ? O1 Nb1 Br4 85.2(3) . . ? Br5 Nb1 Br4 93.44(9) . . ? O1 Nb1 Br1 87.6(3) . . ? Br5 Nb1 Br1 96.75(8) . . ? Br4 Nb1 Br1 87.42(9) . . ? O1 Nb1 Br3 80.5(3) . . ? Br5 Nb1 Br3 95.16(9) . . ? Br4 Nb1 Br3 90.83(9) . . ? Br1 Nb1 Br3 168.04(9) . . ? O1 Nb1 Br2 85.9(3) . . ? Br5 Nb1 Br2 95.68(8) . . ? Br4 Nb1 Br2 170.66(10) . . ? Br1 Nb1 Br2 89.51(8) . . ? Br3 Nb1 Br2 90.34(9) . . ? O1 Nb2 O3 163.7(5) . . ? O1 Nb2 O2 93.2(5) . . ? O3 Nb2 O2 70.8(4) . . ? O1 Nb2 Br6 102.2(4) . . ? O3 Nb2 Br6 94.0(3) . . ? O2 Nb2 Br6 164.3(3) . . ? O1 Nb2 Br7 94.8(4) . . ? O3 Nb2 Br7 80.8(4) . . ? O2 Nb2 Br7 83.2(3) . . ? Br6 Nb2 Br7 98.22(9) . . ? O1 Nb2 Br8 97.1(4) . . ? O3 Nb2 Br8 83.4(4) . . ? O2 Nb2 Br8 80.1(3) . . ? Br6 Nb2 Br8 94.92(9) . . ? Br7 Nb2 Br8 160.02(10) . . ? O2 C1 H1A 109.5 . . ? O2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C2 C3 107.1(12) . . ? O2 C2 H2A 110.3 . . ? C3 C2 H2A 110.3 . . ? O2 C2 H2B 110.3 . . ? C3 C2 H2B 110.3 . . ? H2A C2 H2B 108.6 . . ? O3 C3 O4 129.1(15) . . ? O3 C3 C2 119.6(14) . . ? O4 C3 C2 111.2(14) . . ? O4 C4 H4A 109.5 . . ? O4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Nb2 O1 Nb1 171.8(7) . . ? C1 O2 C2 111.5(12) . . ? C1 O2 Nb2 122.8(9) . . ? C2 O2 Nb2 119.5(9) . . ? C3 O3 Nb2 121.6(10) . . ? C3 O4 C4 117.7(13) . . ? 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 O2 C2 C3 O3 -14(2) . . . . ? O2 C2 C3 O4 169.5(13) . . . . ? O3 Nb2 O1 Nb1 154(4) . . . . ? O2 Nb2 O1 Nb1 164(5) . . . . ? Br6 Nb2 O1 Nb1 -19(5) . . . . ? Br7 Nb2 O1 Nb1 81(5) . . . . ? Br8 Nb2 O1 Nb1 -115(5) . . . . ? Br5 Nb1 O1 Nb2 115(5) . . . . ? Br4 Nb1 O1 Nb2 42(5) . . . . ? Br1 Nb1 O1 Nb2 -46(5) . . . . ? Br3 Nb1 O1 Nb2 134(5) . . . . ? Br2 Nb1 O1 Nb2 -135(5) . . . . ? C3 C2 O2 C1 161.1(13) . . . . ? C3 C2 O2 Nb2 8.1(16) . . . . ? O1 Nb2 O2 C1 31.1(12) . . . . ? O3 Nb2 O2 C1 -151.9(13) . . . . ? Br6 Nb2 O2 C1 -138.2(11) . . . . ? Br7 Nb2 O2 C1 125.6(12) . . . . ? Br8 Nb2 O2 C1 -65.5(11) . . . . ? O1 Nb2 O2 C2 -179.1(11) . . . . ? O3 Nb2 O2 C2 -2.0(10) . . . . ? Br6 Nb2 O2 C2 11.7(19) . . . . ? Br7 Nb2 O2 C2 -84.6(10) . . . . ? Br8 Nb2 O2 C2 84.3(10) . . . . ? O4 C3 O3 Nb2 -170.2(13) . . . . ? C2 C3 O3 Nb2 14(2) . . . . ? O1 Nb2 O3 C3 4(3) . . . . ? O2 Nb2 O3 C3 -6.7(13) . . . . ? Br6 Nb2 O3 C3 177.0(13) . . . . ? Br7 Nb2 O3 C3 79.3(13) . . . . ? Br8 Nb2 O3 C3 -88.5(14) . . . . ? O3 C3 O4 C4 4(3) . . . . ? C2 C3 O4 C4 -179.9(13) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.785 _refine_diff_density_min -3.000 _refine_diff_density_rms 0.379 # Attachment 'Compound_3a.CIF' data_pbca _database_code_depnum_ccdc_archive 'CCDC 723066' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 Cl8 Nb2 O4' _chemical_formula_weight 589.52 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' 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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.4931(6) _cell_length_b 15.0005(8) _cell_length_c 19.9805(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3444.7(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9851 _cell_measurement_theta_min 2.454 _cell_measurement_theta_max 28.6375 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 2.570 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6144 _exptl_absorpt_correction_T_max 0.7653 _exptl_absorpt_process_details 'SADABS (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37525 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0125 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 28.00 _reflns_number_total 4139 _reflns_number_gt 3889 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0159P)^2^+2.1847P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4139 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0184 _refine_ls_R_factor_gt 0.0164 _refine_ls_wR_factor_ref 0.0376 _refine_ls_wR_factor_gt 0.0369 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.005 _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 C1 C 0.78651(14) 0.35749(11) 0.64319(9) 0.0209(3) Uani 1 1 d . . . H1A H 0.8115 0.2966 0.6328 0.031 Uiso 1 1 calc R . . H1B H 0.7169 0.3720 0.6170 0.031 Uiso 1 1 calc R . . H1C H 0.7686 0.3621 0.6910 0.031 Uiso 1 1 calc R . . C2 C 0.84549(14) 0.50957(11) 0.64105(9) 0.0196(3) Uani 1 1 d . . . H2A H 0.8110 0.5131 0.6864 0.024 Uiso 1 1 calc R . . H2B H 0.7870 0.5304 0.6082 0.024 Uiso 1 1 calc R . . C3 C 0.95309(14) 0.56579(11) 0.63713(8) 0.0169(3) Uani 1 1 d . . . C4 C 1.03469(16) 0.70959(12) 0.63011(9) 0.0246(4) Uani 1 1 d . . . H4A H 1.0088 0.7718 0.6306 0.037 Uiso 1 1 calc R . . H4B H 1.0745 0.6971 0.5878 0.037 Uiso 1 1 calc R . . H4C H 1.0883 0.6993 0.6675 0.037 Uiso 1 1 calc R . . Cl1 Cl 1.16103(4) 0.15879(3) 0.52709(2) 0.02329(9) Uani 1 1 d . . . Cl2 Cl 0.87402(3) 0.17131(3) 0.53350(2) 0.02083(8) Uani 1 1 d . . . Cl3 Cl 0.88673(4) 0.13509(3) 0.69663(2) 0.02048(8) Uani 1 1 d . . . Cl4 Cl 1.16863(4) 0.11779(3) 0.68748(2) 0.02261(9) Uani 1 1 d . . . Cl5 Cl 1.00099(4) -0.01648(2) 0.588073(19) 0.01826(8) Uani 1 1 d . . . Cl6 Cl 1.26413(3) 0.37563(3) 0.65522(2) 0.02212(9) Uani 1 1 d . . . Cl7 Cl 1.02624(3) 0.40061(3) 0.75002(2) 0.02003(8) Uani 1 1 d . . . Cl8 Cl 1.08726(4) 0.40818(3) 0.52100(2) 0.02406(9) Uani 1 1 d . . . Nb1 Nb 1.021107(12) 0.131517(9) 0.608340(7) 0.01138(4) Uani 1 1 d . . . Nb2 Nb 1.069399(11) 0.383552(9) 0.635536(7) 0.01132(4) Uani 1 1 d . . . O1 O 1.03192(9) 0.27077(8) 0.62812(6) 0.0155(2) Uani 1 1 d . . . O2 O 0.87987(9) 0.41998(7) 0.62638(5) 0.0156(2) Uani 1 1 d . . . O3 O 1.05001(10) 0.53093(8) 0.63496(6) 0.0176(2) Uani 1 1 d . . . O4 O 0.93342(11) 0.65050(8) 0.63679(6) 0.0206(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0120(7) 0.0214(8) 0.0293(9) -0.0028(7) 0.0016(6) -0.0021(6) C2 0.0178(8) 0.0179(8) 0.0231(8) -0.0011(6) 0.0029(6) 0.0070(6) C3 0.0222(8) 0.0171(8) 0.0114(7) -0.0008(6) 0.0006(6) 0.0041(6) C4 0.0313(10) 0.0147(8) 0.0278(10) 0.0013(7) -0.0009(7) -0.0008(7) Cl1 0.0232(2) 0.0259(2) 0.0208(2) -0.00416(16) 0.00954(15) -0.00661(16) Cl2 0.02132(19) 0.02237(19) 0.01881(19) -0.00170(15) -0.00799(15) 0.00341(16) Cl3 0.02018(19) 0.0244(2) 0.01684(18) -0.00299(15) 0.00657(15) -0.00627(15) Cl4 0.02012(19) 0.0255(2) 0.0222(2) 0.00021(15) -0.00957(15) -0.00047(16) Cl5 0.02550(19) 0.01304(17) 0.01625(18) -0.00091(13) -0.00179(15) -0.00194(15) Cl6 0.01156(17) 0.0233(2) 0.0315(2) 0.00027(16) -0.00231(15) -0.00112(15) Cl7 0.0237(2) 0.02358(19) 0.01276(17) -0.00223(15) 0.00063(14) 0.00134(15) Cl8 0.0316(2) 0.0264(2) 0.01414(18) 0.00351(15) 0.00441(16) 0.01031(17) Nb1 0.01158(7) 0.01238(7) 0.01017(7) -0.00066(5) -0.00038(5) -0.00171(5) Nb2 0.01058(7) 0.01106(7) 0.01232(7) -0.00059(5) -0.00011(5) 0.00033(5) O1 0.0144(5) 0.0155(5) 0.0166(5) -0.0022(4) 0.0006(4) -0.0011(4) O2 0.0122(5) 0.0153(5) 0.0193(6) -0.0024(4) 0.0009(4) 0.0018(4) O3 0.0174(5) 0.0148(5) 0.0205(6) -0.0004(4) -0.0005(5) 0.0022(4) O4 0.0249(6) 0.0148(5) 0.0220(6) -0.0004(5) 0.0011(5) 0.0049(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 C1 O2 1.4639(19) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O2 1.4311(19) . ? C2 C3 1.499(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O3 1.231(2) . ? C3 O4 1.291(2) . ? C4 O4 1.469(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? Cl1 Nb1 2.3215(4) . ? Cl2 Nb1 2.3346(4) . ? Cl3 Nb1 2.3452(4) . ? Cl4 Nb1 2.3275(4) . ? Cl5 Nb1 2.2684(4) . ? Cl6 Nb2 2.2755(4) . ? Cl7 Nb2 2.3546(4) . ? Cl8 Nb2 2.3271(4) . ? Nb1 O1 2.1296(11) . ? Nb2 O1 1.7520(11) . ? Nb2 O3 2.2220(12) . ? Nb2 O2 2.2532(11) . ? 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 C1 H1A 109.5 . . ? O2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C2 C3 106.85(13) . . ? O2 C2 H2A 110.4 . . ? C3 C2 H2A 110.4 . . ? O2 C2 H2B 110.4 . . ? C3 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? O3 C3 O4 125.20(16) . . ? O3 C3 C2 120.61(15) . . ? O4 C3 C2 114.19(14) . . ? O4 C4 H4A 109.5 . . ? O4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O1 Nb1 Cl5 177.47(3) . . ? O1 Nb1 Cl1 85.21(3) . . ? Cl5 Nb1 Cl1 96.791(15) . . ? O1 Nb1 Cl4 85.31(3) . . ? Cl5 Nb1 Cl4 96.255(15) . . ? Cl1 Nb1 Cl4 89.202(17) . . ? O1 Nb1 Cl2 84.86(3) . . ? Cl5 Nb1 Cl2 93.557(15) . . ? Cl1 Nb1 Cl2 90.493(17) . . ? Cl4 Nb1 Cl2 170.150(16) . . ? O1 Nb1 Cl3 82.90(3) . . ? Cl5 Nb1 Cl3 95.135(15) . . ? Cl1 Nb1 Cl3 168.015(16) . . ? Cl4 Nb1 Cl3 88.322(16) . . ? Cl2 Nb1 Cl3 89.949(16) . . ? O1 Nb2 O3 159.33(5) . . ? O1 Nb2 O2 89.40(5) . . ? O3 Nb2 O2 70.20(4) . . ? O1 Nb2 Cl6 101.89(4) . . ? O3 Nb2 Cl6 98.71(3) . . ? O2 Nb2 Cl6 167.84(3) . . ? O1 Nb2 Cl8 95.27(4) . . ? O3 Nb2 Cl8 81.13(3) . . ? O2 Nb2 Cl8 88.11(3) . . ? Cl6 Nb2 Cl8 95.250(17) . . ? O1 Nb2 Cl7 97.78(4) . . ? O3 Nb2 Cl7 82.86(3) . . ? O2 Nb2 Cl7 81.30(3) . . ? Cl6 Nb2 Cl7 92.578(16) . . ? Cl8 Nb2 Cl7 163.072(16) . . ? Nb2 O1 Nb1 167.74(6) . . ? C2 O2 C1 110.61(12) . . ? C2 O2 Nb2 118.55(9) . . ? C1 O2 Nb2 122.32(9) . . ? C3 O3 Nb2 120.87(11) . . ? C3 O4 C4 117.11(13) . . ? 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 O2 C2 C3 O3 -12.7(2) . . . . ? O2 C2 C3 O4 167.71(13) . . . . ? O3 Nb2 O1 Nb1 137.0(3) . . . . ? O2 Nb2 O1 Nb1 146.2(3) . . . . ? Cl6 Nb2 O1 Nb1 -38.3(3) . . . . ? Cl8 Nb2 O1 Nb1 58.2(3) . . . . ? Cl7 Nb2 O1 Nb1 -132.6(3) . . . . ? Cl5 Nb1 O1 Nb2 -161.5(5) . . . . ? Cl1 Nb1 O1 Nb2 -19.2(3) . . . . ? Cl4 Nb1 O1 Nb2 70.4(3) . . . . ? Cl2 Nb1 O1 Nb2 -110.2(3) . . . . ? Cl3 Nb1 O1 Nb2 159.3(3) . . . . ? C3 C2 O2 C1 167.63(13) . . . . ? C3 C2 O2 Nb2 18.86(16) . . . . ? O1 Nb2 O2 C2 168.66(11) . . . . ? O3 Nb2 O2 C2 -14.79(10) . . . . ? Cl6 Nb2 O2 C2 10.3(2) . . . . ? Cl8 Nb2 O2 C2 -96.05(10) . . . . ? Cl7 Nb2 O2 C2 70.70(10) . . . . ? O1 Nb2 O2 C1 23.72(11) . . . . ? O3 Nb2 O2 C1 -159.73(12) . . . . ? Cl6 Nb2 O2 C1 -134.66(14) . . . . ? Cl8 Nb2 O2 C1 119.01(11) . . . . ? Cl7 Nb2 O2 C1 -74.24(11) . . . . ? O4 C3 O3 Nb2 -179.76(12) . . . . ? C2 C3 O3 Nb2 0.7(2) . . . . ? O1 Nb2 O3 C3 17.2(2) . . . . ? O2 Nb2 O3 C3 7.37(11) . . . . ? Cl6 Nb2 O3 C3 -167.45(11) . . . . ? Cl8 Nb2 O3 C3 98.55(12) . . . . ? Cl7 Nb2 O3 C3 -75.92(12) . . . . ? O3 C3 O4 C4 3.0(2) . . . . ? C2 C3 O4 C4 -177.44(14) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.409 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.161 # Attachment 'Compound_3a1.CIF' data_pca21a _database_code_depnum_ccdc_archive 'CCDC 723067' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 Cl8 Nb2 O4' _chemical_formula_weight 589.52 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' 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 Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 13.7903(19) _cell_length_b 9.5260(13) _cell_length_c 13.3244(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1750.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3746 _cell_measurement_theta_min 2.5985 _cell_measurement_theta_max 25.390 _exptl_crystal_description prism _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 2.529 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6878 _exptl_absorpt_correction_T_max 0.7684 _exptl_absorpt_process_details 'SADABS (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11832 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3083 _reflns_number_gt 2474 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+11.6333P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.08(14) _refine_ls_number_reflns 3083 _refine_ls_number_parameters 233 _refine_ls_number_restraints 290 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.043 _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 -0.00234(7) 0.39635(8) 0.70170(8) 0.0227(2) Uani 1 1 d U A . Cl1 Cl -0.14729(17) 0.2738(3) 0.68147(19) 0.0302(6) Uani 1 1 d U . . Cl2 Cl 0.15580(18) 0.4801(3) 0.7080(2) 0.0375(6) Uani 1 1 d U . . Cl3 Cl 0.0281(2) 0.2639(3) 0.8445(2) 0.0422(8) Uani 1 1 d U . . Cl4 Cl -0.0211(2) 0.4908(4) 0.5423(2) 0.0445(7) Uani 1 1 d U . . Cl5 Cl -0.0700(2) 0.5809(3) 0.7828(2) 0.0450(8) Uani 1 1 d U . . O1 O 0.0600(5) 0.2235(7) 0.6227(6) 0.0312(13) Uani 1 1 d U . . Nb2 Nb 0.14147(12) 0.12182(17) 0.54553(13) 0.0195(5) Uani 0.507(2) 1 d PU A 1 Cl6 Cl 0.0445(12) 0.0916(19) 0.4051(7) 0.031(2) Uani 0.507(2) 1 d PU A 1 Cl7 Cl 0.2401(4) 0.0726(6) 0.6857(4) 0.0340(12) Uani 0.507(2) 1 d PU A 1 Cl8 Cl 0.2496(4) 0.2700(5) 0.4752(4) 0.0287(12) Uani 0.507(2) 1 d PU A 1 C1 C 0.1863(5) -0.1878(7) 0.5069(5) 0.0269(14) Uani 0.507(2) 1 d PGU A 1 C2 C 0.0944(6) -0.2061(8) 0.5696(8) 0.0298(16) Uani 0.507(2) 1 d PGU A 1 H2A H 0.0415 -0.2446 0.5277 0.036 Uiso 0.507(2) 1 calc PR A 1 H2B H 0.1065 -0.2717 0.6258 0.036 Uiso 0.507(2) 1 calc PR A 1 C3 C -0.0314(8) -0.0666(14) 0.6389(12) 0.032(3) Uani 0.507(2) 1 d PGU A 1 H3A H -0.0472 0.0273 0.6643 0.048 Uiso 0.507(2) 1 calc PR A 1 H3B H -0.0416 -0.1359 0.6922 0.048 Uiso 0.507(2) 1 calc PR A 1 H3C H -0.0734 -0.0887 0.5817 0.048 Uiso 0.507(2) 1 calc PR A 1 C4 C 0.3119(7) -0.3035(11) 0.4229(9) 0.030(3) Uani 0.507(2) 1 d PGU A 1 H4A H 0.3330 -0.4001 0.4102 0.045 Uiso 0.507(2) 1 calc PR A 1 H4B H 0.3630 -0.2530 0.4591 0.045 Uiso 0.507(2) 1 calc PR A 1 H4C H 0.2990 -0.2563 0.3589 0.045 Uiso 0.507(2) 1 calc PR A 1 O2 O 0.2108(7) -0.0685(7) 0.4816(9) 0.0275(13) Uani 0.507(2) 1 d PGU A 1 O3 O 0.0681(7) -0.0699(10) 0.6075(8) 0.0286(14) Uani 0.507(2) 1 d PGU A 1 O4 O 0.2237(6) -0.3050(7) 0.4833(8) 0.0263(17) Uani 0.507(2) 1 d PGU A 1 Nb2' Nb 0.08859(12) 0.04522(17) 0.59626(13) 0.0180(5) Uani 0.493(2) 1 d PU A 2 Cl6' Cl 0.1834(4) -0.0046(6) 0.7349(4) 0.0354(13) Uani 0.493(2) 1 d PU A 2 Cl7' Cl 0.0323(11) 0.0791(19) 0.4306(7) 0.0255(19) Uani 0.493(2) 1 d PU A 2 Cl8' Cl -0.0423(4) -0.0878(6) 0.6426(5) 0.0301(12) Uani 0.493(2) 1 d PU A 2 C1' C 0.2341(4) -0.1239(7) 0.4797(5) 0.0261(15) Uani 0.493(2) 1 d PGU A 2 C2' C 0.2826(5) 0.0199(7) 0.4724(6) 0.0280(17) Uani 0.493(2) 1 d PGDU A 2 H2'1 H 0.3456 0.0189 0.5079 0.034 Uiso 0.493(2) 1 calc PR A 2 H2'2 H 0.2943 0.0447 0.4013 0.034 Uiso 0.493(2) 1 calc PR A 2 C3' C 0.2684(7) 0.2469(7) 0.5443(8) 0.047(3) Uani 0.493(2) 1 d PGDU A 2 H3'1 H 0.2228 0.3130 0.5751 0.070 Uiso 0.493(2) 1 calc PR A 2 H3'2 H 0.2963 0.2890 0.4837 0.070 Uiso 0.493(2) 1 calc PR A 2 H3'3 H 0.3204 0.2251 0.5920 0.070 Uiso 0.493(2) 1 calc PR A 2 C4' C 0.2400(8) -0.3583(7) 0.4279(9) 0.025(3) Uani 0.493(2) 1 d PGU A 2 H4'1 H 0.2805 -0.4180 0.3851 0.038 Uiso 0.493(2) 1 calc PR A 2 H4'2 H 0.1734 -0.3578 0.4021 0.038 Uiso 0.493(2) 1 calc PR A 2 H4'3 H 0.2403 -0.3951 0.4966 0.038 Uiso 0.493(2) 1 calc PR A 2 O2' O 0.1644(6) -0.1385(8) 0.5366(8) 0.0268(14) Uani 0.493(2) 1 d PGU A 2 O3' O 0.2182(5) 0.1202(7) 0.5180(6) 0.0272(14) Uani 0.493(2) 1 d PGU A 2 O4' O 0.2782(6) -0.2156(8) 0.4277(7) 0.0257(16) Uani 0.493(2) 1 d PGU A 2 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 0.0276(4) 0.0221(4) 0.0184(4) -0.0055(4) -0.0059(4) 0.0066(4) Cl1 0.0217(11) 0.0380(14) 0.0310(16) -0.0062(11) -0.0037(11) 0.0057(10) Cl2 0.0365(13) 0.0333(13) 0.0428(15) -0.0068(14) -0.0107(14) -0.0101(11) Cl3 0.058(2) 0.0310(15) 0.0377(16) 0.0120(12) -0.0267(14) -0.0071(13) Cl4 0.0393(16) 0.069(2) 0.0251(13) 0.0117(14) -0.0013(13) 0.0068(14) Cl5 0.070(2) 0.0225(13) 0.0430(16) -0.0077(12) 0.0233(16) 0.0059(13) O1 0.017(3) 0.030(2) 0.047(3) -0.021(2) -0.006(2) 0.004(2) Nb2 0.0188(8) 0.0189(9) 0.0208(9) 0.0000(8) 0.0038(7) 0.0017(7) Cl6 0.038(5) 0.028(4) 0.026(4) 0.001(4) -0.006(4) -0.001(3) Cl7 0.028(2) 0.052(3) 0.023(2) -0.002(2) -0.0016(19) 0.015(2) Cl8 0.023(2) 0.020(2) 0.044(3) 0.000(2) 0.009(2) -0.0037(19) C1 0.029(3) 0.023(2) 0.029(3) 0.002(3) 0.003(3) 0.002(2) C2 0.034(3) 0.024(3) 0.032(4) 0.004(3) 0.006(3) 0.001(3) C3 0.032(5) 0.026(6) 0.037(7) 0.001(6) 0.012(5) -0.006(4) C4 0.031(5) 0.029(6) 0.031(6) 0.002(5) 0.006(5) -0.003(5) O2 0.030(3) 0.021(3) 0.031(3) 0.000(3) 0.003(2) 0.003(2) O3 0.031(3) 0.024(3) 0.031(3) 0.004(3) 0.008(3) 0.001(3) O4 0.027(4) 0.024(3) 0.028(4) 0.006(3) 0.002(3) 0.002(3) Nb2' 0.0171(9) 0.0157(9) 0.0211(9) 0.0001(8) 0.0048(7) 0.0007(7) Cl6' 0.033(3) 0.047(3) 0.026(2) -0.004(2) -0.005(2) 0.012(2) Cl7' 0.028(4) 0.027(4) 0.022(4) 0.001(3) 0.006(3) -0.002(3) Cl8' 0.029(2) 0.029(3) 0.032(3) 0.003(2) 0.008(2) -0.007(2) C1' 0.026(3) 0.023(3) 0.029(3) 0.001(3) 0.002(3) 0.005(3) C2' 0.028(3) 0.025(3) 0.031(4) -0.001(3) 0.007(3) 0.003(3) C3' 0.042(6) 0.028(5) 0.071(7) -0.008(6) 0.012(6) -0.012(4) C4' 0.025(6) 0.024(4) 0.027(6) 0.002(5) -0.004(6) 0.000(5) O2' 0.028(3) 0.022(3) 0.030(3) -0.001(3) 0.005(3) 0.003(2) O3' 0.025(3) 0.023(3) 0.034(3) -0.003(3) 0.009(2) -0.002(3) O4' 0.026(3) 0.024(3) 0.026(3) 0.003(3) 0.003(3) 0.001(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 2.135(7) . ? Nb1 Cl5 2.265(3) . ? Nb1 Cl3 2.321(3) . ? Nb1 Cl4 2.322(3) . ? Nb1 Cl2 2.324(3) . ? Nb1 Cl1 2.331(3) . ? O1 Nb2' 1.779(7) . ? O1 Nb2 1.805(7) . ? Nb2 O2 2.219(8) . ? Nb2 O3 2.245(10) . ? Nb2 Cl8 2.257(5) . ? Nb2 Cl6 2.317(12) . ? Nb2 Cl7 2.357(5) . ? C1 O2 1.2331 . ? C1 O4 1.2702 . ? C1 C2 1.5269 . ? C2 O3 1.4390 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O3 1.4345 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 O4 1.4580 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? Nb2' O2' 2.188(8) . ? Nb2' O3' 2.190(9) . ? Nb2' Cl8' 2.290(6) . ? Nb2' Cl6' 2.312(5) . ? Nb2' Cl7' 2.362(10) . ? C1' O2' 1.2331 . ? C1' O4' 1.2702 . ? C1' C2' 1.5269 . ? C2' O3' 1.4390 . ? C2' H2'1 0.9900 . ? C2' H2'2 0.9900 . ? C3' O3' 1.4345 . ? C3' H3'1 0.9800 . ? C3' H3'2 0.9800 . ? C3' H3'3 0.9800 . ? C4' O4' 1.4581 . ? C4' H4'1 0.9800 . ? C4' H4'2 0.9800 . ? C4' H4'3 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 Cl5 178.9(2) . . ? O1 Nb1 Cl3 84.9(2) . . ? Cl5 Nb1 Cl3 96.06(12) . . ? O1 Nb1 Cl4 83.9(2) . . ? Cl5 Nb1 Cl4 95.14(12) . . ? Cl3 Nb1 Cl4 168.79(12) . . ? O1 Nb1 Cl2 84.51(19) . . ? Cl5 Nb1 Cl2 95.91(11) . . ? Cl3 Nb1 Cl2 89.26(11) . . ? Cl4 Nb1 Cl2 90.27(12) . . ? O1 Nb1 Cl1 84.39(18) . . ? Cl5 Nb1 Cl1 95.21(11) . . ? Cl3 Nb1 Cl1 88.73(10) . . ? Cl4 Nb1 Cl1 89.58(10) . . ? Cl2 Nb1 Cl1 168.85(10) . . ? Nb2' O1 Nb2 40.26(16) . . ? Nb2' O1 Nb1 157.4(4) . . ? Nb2 O1 Nb1 161.0(4) . . ? O1 Nb2 O2 157.7(3) . . ? O1 Nb2 O3 86.9(3) . . ? O2 Nb2 O3 70.8(2) . . ? O1 Nb2 Cl8 108.2(3) . . ? O2 Nb2 Cl8 93.8(2) . . ? O3 Nb2 Cl8 163.6(2) . . ? O1 Nb2 Cl6 99.7(5) . . ? O2 Nb2 Cl6 80.6(6) . . ? O3 Nb2 Cl6 86.3(4) . . ? Cl8 Nb2 Cl6 97.1(3) . . ? O1 Nb2 Cl7 90.8(3) . . ? O2 Nb2 Cl7 83.9(4) . . ? O3 Nb2 Cl7 78.9(3) . . ? Cl8 Nb2 Cl7 94.2(2) . . ? Cl6 Nb2 Cl7 161.4(5) . . ? O2 C1 O4 129.1 . . ? O2 C1 C2 118.8 . . ? O4 C1 C2 111.9 . . ? O3 C2 C1 107.4 . . ? O3 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? O3 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? O3 C3 H3A 109.5 . . ? O3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O4 C4 H4A 109.5 . . ? O4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 O2 Nb2 122.0(3) . . ? C3 O3 C2 111.3 . . ? C3 O3 Nb2 121.4(3) . . ? C2 O3 Nb2 119.4(3) . . ? C1 O4 C4 117.9 . . ? O1 Nb2' O2' 160.3(3) . . ? O1 Nb2' O3' 87.9(3) . . ? O2' Nb2' O3' 72.42(19) . . ? O1 Nb2' Cl8' 107.5(3) . . ? O2' Nb2' Cl8' 91.8(2) . . ? O3' Nb2' Cl8' 162.3(3) . . ? O1 Nb2' Cl6' 99.4(3) . . ? O2' Nb2' Cl6' 81.7(4) . . ? O3' Nb2' Cl6' 89.2(2) . . ? Cl8' Nb2' Cl6' 96.7(2) . . ? O1 Nb2' Cl7' 89.0(5) . . ? O2' Nb2' Cl7' 85.8(6) . . ? O3' Nb2' Cl7' 77.2(4) . . ? Cl8' Nb2' Cl7' 93.9(4) . . ? Cl6' Nb2' Cl7' 163.8(4) . . ? O2' C1' O4' 129.1 . . ? O2' C1' C2' 118.8 . . ? O4' C1' C2' 111.9 . . ? O3' C2' C1' 107.4 . . ? O3' C2' H2'1 110.2 . . ? C1' C2' H2'1 110.2 . . ? O3' C2' H2'2 110.2 . . ? C1' C2' H2'2 110.2 . . ? H2'1 C2' H2'2 108.5 . . ? O3' C3' H3'1 109.5 . . ? O3' C3' H3'2 109.5 . . ? H3'1 C3' H3'2 109.5 . . ? O3' C3' H3'3 109.5 . . ? H3'1 C3' H3'3 109.5 . . ? H3'2 C3' H3'3 109.5 . . ? O4' C4' H4'1 109.5 . . ? O4' C4' H4'2 109.5 . . ? H4'1 C4' H4'2 109.5 . . ? O4' C4' H4'3 109.5 . . ? H4'1 C4' H4'3 109.5 . . ? H4'2 C4' H4'3 109.5 . . ? C1' O2' Nb2' 120.4(3) . . ? C3' O3' C2' 111.3 . . ? C3' O3' Nb2' 123.5(3) . . ? C2' O3' Nb2' 119.2(3) . . ? C1' O4' C4' 117.9 . . ? 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 Cl5 Nb1 O1 Nb2' -123(11) . . . . ? Cl3 Nb1 O1 Nb2' 34.6(10) . . . . ? Cl4 Nb1 O1 Nb2' -144.8(10) . . . . ? Cl2 Nb1 O1 Nb2' 124.3(10) . . . . ? Cl1 Nb1 O1 Nb2' -54.7(10) . . . . ? Cl5 Nb1 O1 Nb2 86(11) . . . . ? Cl3 Nb1 O1 Nb2 -116.8(13) . . . . ? Cl4 Nb1 O1 Nb2 63.8(13) . . . . ? Cl2 Nb1 O1 Nb2 -27.0(13) . . . . ? Cl1 Nb1 O1 Nb2 154.0(13) . . . . ? Nb2' O1 Nb2 O2 -0.9(11) . . . . ? Nb1 O1 Nb2 O2 162.6(12) . . . . ? Nb2' O1 Nb2 O3 2.2(3) . . . . ? Nb1 O1 Nb2 O3 165.7(13) . . . . ? Nb2' O1 Nb2 Cl8 -171.2(2) . . . . ? Nb1 O1 Nb2 Cl8 -7.8(14) . . . . ? Nb2' O1 Nb2 Cl6 87.9(4) . . . . ? Nb1 O1 Nb2 Cl6 -108.6(13) . . . . ? Nb2' O1 Nb2 Cl7 -76.6(2) . . . . ? Nb1 O1 Nb2 Cl7 86.8(13) . . . . ? O2 C1 C2 O3 -14.4 . . . . ? O4 C1 C2 O3 169.7 . . . . ? O4 C1 O2 Nb2 -173.9(7) . . . . ? C2 C1 O2 Nb2 11.0(7) . . . . ? O1 Nb2 O2 C1 0.2(17) . . . . ? O3 Nb2 O2 C1 -3.1(8) . . . . ? Cl8 Nb2 O2 C1 171.0(8) . . . . ? Cl6 Nb2 O2 C1 -92.4(9) . . . . ? Cl7 Nb2 O2 C1 77.3(8) . . . . ? C1 C2 O3 C3 161.2 . . . . ? C1 C2 O3 Nb2 11.8(7) . . . . ? O1 Nb2 O3 C3 29.1(4) . . . . ? O2 Nb2 O3 C3 -152.16(12) . . . . ? Cl8 Nb2 O3 C3 -173.4(12) . . . . ? Cl6 Nb2 O3 C3 -70.8(5) . . . . ? Cl7 Nb2 O3 C3 120.5(3) . . . . ? O1 Nb2 O3 C2 175.4(6) . . . . ? O2 Nb2 O3 C2 -5.9(8) . . . . ? Cl8 Nb2 O3 C2 -27.1(15) . . . . ? Cl6 Nb2 O3 C2 75.5(7) . . . . ? Cl7 Nb2 O3 C2 -93.2(5) . . . . ? O2 C1 O4 C4 4.4 . . . . ? C2 C1 O4 C4 179.8 . . . . ? Nb2 O1 Nb2' O2' 9.1(12) . . . . ? Nb1 O1 Nb2' O2' -157.0(11) . . . . ? Nb2 O1 Nb2' O3' 11.8(2) . . . . ? Nb1 O1 Nb2' O3' -154.2(10) . . . . ? Nb2 O1 Nb2' Cl8' -159.3(2) . . . . ? Nb1 O1 Nb2' Cl8' 34.7(11) . . . . ? Nb2 O1 Nb2' Cl6' 100.6(2) . . . . ? Nb1 O1 Nb2' Cl6' -65.4(10) . . . . ? Nb2 O1 Nb2' Cl7' -65.4(4) . . . . ? Nb1 O1 Nb2' Cl7' 128.5(10) . . . . ? O2' C1' C2' O3' -14.4 . . . . ? O4' C1' C2' O3' 169.7 . . . . ? O4' C1' O2' Nb2' -169.5(6) . . . . ? C2' C1' O2' Nb2' 15.4(6) . . . . ? O1 Nb2' O2' C1' -5.3(18) . . . . ? O3' Nb2' O2' C1' -8.1(7) . . . . ? Cl8' Nb2' O2' C1' 163.6(7) . . . . ? Cl6' Nb2' O2' C1' -99.9(7) . . . . ? Cl7' Nb2' O2' C1' 69.8(8) . . . . ? C1' C2' O3' C3' 161.2 . . . . ? C1' C2' O3' Nb2' 7.3(6) . . . . ? O1 Nb2' O3' C3' 29.6(4) . . . . ? O2' Nb2' O3' C3' -151.40(11) . . . . ? Cl8' Nb2' O3' C3' -179.6(9) . . . . ? Cl6' Nb2' O3' C3' -69.8(3) . . . . ? Cl7' Nb2' O3' C3' 119.0(5) . . . . ? O1 Nb2' O3' C2' -179.9(5) . . . . ? O2' Nb2' O3' C2' -0.9(7) . . . . ? Cl8' Nb2' O3' C2' -29.0(12) . . . . ? Cl6' Nb2' O3' C2' 80.7(5) . . . . ? Cl7' Nb2' O3' C2' -90.5(7) . . . . ? O2' C1' O4' C4' 4.4 . . . . ? C2' C1' O4' C4' 179.8 . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.239 _refine_diff_density_min -1.142 _refine_diff_density_rms 0.162 # Attachment 'Compound_7.CIF' data_p-1 _database_code_depnum_ccdc_archive 'CCDC 723068' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 Cl8 Nb2 O5' _chemical_formula_weight 629.54 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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6101(11) _cell_length_b 10.2922(15) _cell_length_c 12.5072(18) _cell_angle_alpha 87.334(2) _cell_angle_beta 80.106(2) _cell_angle_gamma 76.815(2) _cell_volume 939.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7582 _cell_measurement_theta_min 2.610 _cell_measurement_theta_max 28.4305 _exptl_crystal_description prism _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 2.367 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6363 _exptl_absorpt_correction_T_max 0.7808 _exptl_absorpt_process_details 'SADABS (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10393 _diffrn_reflns_av_R_equivalents 0.0161 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4062 _reflns_number_gt 3712 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+0.4421P] 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 4062 _refine_ls_number_parameters 198 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0172 _refine_ls_wR_factor_ref 0.0451 _refine_ls_wR_factor_gt 0.0436 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.050 _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 C1 C 0.4777(3) -0.24088(19) 0.34822(15) 0.0180(4) Uani 1 1 d . . . C2 C 0.6395(3) -0.2744(2) 0.26192(18) 0.0239(4) Uani 1 1 d D . . H2 H 0.684(3) -0.3651(10) 0.2539(19) 0.029 Uiso 1 1 d D . . C3 C 0.7249(3) -0.1941(2) 0.19713(18) 0.0237(4) Uani 1 1 d D . . H3 H 0.824(2) -0.231(2) 0.1461(15) 0.028 Uiso 1 1 d D . . C4 C 0.6920(3) -0.04700(19) 0.19312(15) 0.0178(4) Uani 1 1 d . . . C5 C 0.3076(3) -0.3252(2) 0.50027(17) 0.0248(4) Uani 1 1 d . . . H5A H 0.3187 -0.2613 0.5531 0.037 Uiso 1 1 calc R . . H5B H 0.3029 -0.4112 0.5364 0.037 Uiso 1 1 calc R . . H5C H 0.1952 -0.2914 0.4698 0.037 Uiso 1 1 calc R . . C6 C 0.8128(3) 0.13378(19) 0.11232(17) 0.0213(4) Uani 1 1 d . . . H6A H 0.7014 0.1756 0.0834 0.032 Uiso 1 1 calc R . . H6B H 0.9201 0.1479 0.0614 0.032 Uiso 1 1 calc R . . H6C H 0.8102 0.1738 0.1823 0.032 Uiso 1 1 calc R . . Cl1 Cl 0.37261(7) 0.33725(5) 0.02571(4) 0.02698(11) Uani 1 1 d . . . Cl2 Cl 0.48551(7) 0.40195(5) 0.25775(4) 0.02579(11) Uani 1 1 d . . . Cl3 Cl 0.04550(7) 0.48499(5) 0.36184(4) 0.02818(12) Uani 1 1 d . . . Cl4 Cl -0.05965(6) 0.42513(5) 0.13029(4) 0.02149(10) Uani 1 1 d . . . Cl5 Cl 0.20907(7) 0.64698(5) 0.13825(5) 0.03264(13) Uani 1 1 d . . . Cl6 Cl -0.01931(6) 0.04055(5) 0.35808(4) 0.01994(10) Uani 1 1 d . . . Cl7 Cl 0.29493(7) -0.03769(5) 0.12798(4) 0.02089(10) Uani 1 1 d . . . Cl8 Cl 0.32987(7) 0.13329(5) 0.45821(4) 0.02083(10) Uani 1 1 d . . . Nb1 Nb 0.21323(2) 0.430617(16) 0.189342(13) 0.01467(5) Uani 1 1 d . . . Nb2 Nb 0.27149(2) 0.068363(15) 0.294298(13) 0.01281(5) Uani 1 1 d . . . O1 O 0.22315(18) 0.23123(12) 0.24082(10) 0.0164(3) Uani 1 1 d . . . O2 O 0.56327(18) 0.03520(13) 0.24414(11) 0.0183(3) Uani 1 1 d . . . O3 O 0.36328(18) -0.13492(13) 0.35905(11) 0.0180(3) Uani 1 1 d . . . O4 O 0.46539(19) -0.34246(13) 0.41315(11) 0.0206(3) Uani 1 1 d . . . O5 O 0.82318(18) -0.00951(13) 0.12710(11) 0.0193(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0197(10) 0.0164(9) 0.0195(9) -0.0021(7) -0.0058(8) -0.0050(7) C2 0.0229(10) 0.0140(9) 0.0308(11) -0.0039(8) -0.0003(9) 0.0015(8) C3 0.0181(10) 0.0210(10) 0.0279(11) -0.0064(8) 0.0030(8) 0.0001(8) C4 0.0141(9) 0.0215(10) 0.0187(9) -0.0010(7) -0.0044(8) -0.0042(7) C5 0.0260(11) 0.0215(10) 0.0242(10) 0.0025(8) 0.0014(9) -0.0040(8) C6 0.0198(10) 0.0196(10) 0.0235(10) 0.0020(8) -0.0009(8) -0.0046(8) Cl1 0.0222(2) 0.0361(3) 0.0164(2) -0.00226(19) 0.00214(19) 0.0028(2) Cl2 0.0209(2) 0.0257(3) 0.0334(3) -0.0051(2) -0.0087(2) -0.00661(19) Cl3 0.0316(3) 0.0315(3) 0.0188(2) -0.0085(2) 0.0052(2) -0.0068(2) Cl4 0.0169(2) 0.0220(2) 0.0253(2) 0.00118(18) -0.00456(19) -0.00326(18) Cl5 0.0247(3) 0.0174(2) 0.0527(3) 0.0087(2) 0.0017(2) -0.0060(2) Cl6 0.0151(2) 0.0244(2) 0.0201(2) 0.00100(17) -0.00153(17) -0.00530(18) Cl7 0.0241(2) 0.0210(2) 0.0176(2) -0.00523(17) -0.00413(18) -0.00380(18) Cl8 0.0242(2) 0.0216(2) 0.0181(2) -0.00245(17) -0.00756(18) -0.00452(18) Nb1 0.01424(9) 0.01297(9) 0.01550(9) -0.00044(6) 0.00050(6) -0.00249(6) Nb2 0.01287(9) 0.01183(9) 0.01333(8) -0.00044(6) -0.00214(6) -0.00188(6) O1 0.0177(7) 0.0141(6) 0.0166(7) 0.0004(5) -0.0028(5) -0.0023(5) O2 0.0141(7) 0.0180(7) 0.0217(7) -0.0032(5) -0.0002(5) -0.0027(5) O3 0.0180(7) 0.0143(6) 0.0205(7) 0.0003(5) -0.0032(5) -0.0014(5) O4 0.0230(7) 0.0138(7) 0.0233(7) 0.0007(5) -0.0023(6) -0.0018(5) O5 0.0160(7) 0.0210(7) 0.0199(7) -0.0004(5) -0.0015(5) -0.0034(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 C1 O3 1.227(2) . ? C1 O4 1.304(2) . ? C1 C2 1.478(3) . ? C2 C3 1.328(3) . ? C2 H2 0.922(9) . ? C3 C4 1.477(3) . ? C3 H3 0.921(10) . ? C4 O2 1.241(2) . ? C4 O5 1.300(2) . ? C5 O4 1.460(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 O5 1.464(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? Cl1 Nb1 2.3197(6) . ? Cl2 Nb1 2.3280(6) . ? Cl3 Nb1 2.3318(6) . ? Cl4 Nb1 2.3335(6) . ? Cl5 Nb1 2.2827(6) . ? Cl6 Nb2 2.2971(6) . ? Cl7 Nb2 2.3549(5) . ? Cl8 Nb2 2.3286(5) . ? Nb1 O1 2.1106(13) . ? Nb2 O1 1.7582(13) . ? Nb2 O2 2.1532(13) . ? Nb2 O3 2.2117(13) . ? 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 C1 O4 122.23(18) . . ? O3 C1 C2 126.80(18) . . ? O4 C1 C2 110.94(17) . . ? C3 C2 C1 129.59(19) . . ? C3 C2 H2 117.7(15) . . ? C1 C2 H2 112.7(15) . . ? C2 C3 C4 130.60(19) . . ? C2 C3 H3 119.2(15) . . ? C4 C3 H3 110.2(15) . . ? O2 C4 O5 121.57(17) . . ? O2 C4 C3 128.11(17) . . ? O5 C4 C3 110.31(17) . . ? O4 C5 H5A 109.5 . . ? O4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O5 C6 H6A 109.5 . . ? O5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 Nb1 Cl5 177.89(4) . . ? O1 Nb1 Cl1 84.89(4) . . ? Cl5 Nb1 Cl1 95.99(2) . . ? O1 Nb1 Cl2 84.30(4) . . ? Cl5 Nb1 Cl2 93.77(2) . . ? Cl1 Nb1 Cl2 90.54(2) . . ? O1 Nb1 Cl3 84.77(4) . . ? Cl5 Nb1 Cl3 94.41(2) . . ? Cl1 Nb1 Cl3 169.47(2) . . ? Cl2 Nb1 Cl3 90.43(2) . . ? O1 Nb1 Cl4 86.70(4) . . ? Cl5 Nb1 Cl4 95.23(2) . . ? Cl1 Nb1 Cl4 88.93(2) . . ? Cl2 Nb1 Cl4 170.995(19) . . ? Cl3 Nb1 Cl4 88.48(2) . . ? O1 Nb2 O2 95.24(6) . . ? O1 Nb2 O3 173.87(5) . . ? O2 Nb2 O3 78.80(5) . . ? O1 Nb2 Cl6 100.65(4) . . ? O2 Nb2 Cl6 163.85(4) . . ? O3 Nb2 Cl6 85.38(4) . . ? O1 Nb2 Cl8 94.79(4) . . ? O2 Nb2 Cl8 84.75(4) . . ? O3 Nb2 Cl8 83.30(4) . . ? Cl6 Nb2 Cl8 96.727(19) . . ? O1 Nb2 Cl7 95.01(4) . . ? O2 Nb2 Cl7 81.39(4) . . ? O3 Nb2 Cl7 85.58(4) . . ? Cl6 Nb2 Cl7 94.239(18) . . ? Cl8 Nb2 Cl7 163.685(19) . . ? Nb2 O1 Nb1 168.20(8) . . ? C4 O2 Nb2 139.96(12) . . ? C1 O3 Nb2 146.68(13) . . ? C1 O4 C5 116.92(15) . . ? C4 O5 C6 117.94(15) . . ? 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 C1 C2 C3 19.9(4) . . . . ? O4 C1 C2 C3 -162.1(2) . . . . ? C1 C2 C3 C4 3.0(4) . . . . ? C2 C3 C4 O2 -7.7(4) . . . . ? C2 C3 C4 O5 171.2(2) . . . . ? O2 Nb2 O1 Nb1 -40.8(4) . . . . ? O3 Nb2 O1 Nb1 -27.3(8) . . . . ? Cl6 Nb2 O1 Nb1 142.1(4) . . . . ? Cl8 Nb2 O1 Nb1 44.3(4) . . . . ? Cl7 Nb2 O1 Nb1 -122.6(4) . . . . ? Cl5 Nb1 O1 Nb2 -20.0(14) . . . . ? Cl1 Nb1 O1 Nb2 95.0(4) . . . . ? Cl2 Nb1 O1 Nb2 3.9(4) . . . . ? Cl3 Nb1 O1 Nb2 -87.0(4) . . . . ? Cl4 Nb1 O1 Nb2 -175.8(4) . . . . ? O5 C4 O2 Nb2 140.14(16) . . . . ? C3 C4 O2 Nb2 -41.1(3) . . . . ? O1 Nb2 O2 C4 -127.4(2) . . . . ? O3 Nb2 O2 C4 54.04(19) . . . . ? Cl6 Nb2 O2 C4 42.2(3) . . . . ? Cl8 Nb2 O2 C4 138.2(2) . . . . ? Cl7 Nb2 O2 C4 -33.12(19) . . . . ? O4 C1 O3 Nb2 -177.17(14) . . . . ? C2 C1 O3 Nb2 0.5(4) . . . . ? O1 Nb2 O3 C1 -43.9(6) . . . . ? O2 Nb2 O3 C1 -30.2(2) . . . . ? Cl6 Nb2 O3 C1 146.5(2) . . . . ? Cl8 Nb2 O3 C1 -116.2(2) . . . . ? Cl7 Nb2 O3 C1 51.8(2) . . . . ? O3 C1 O4 C5 0.2(3) . . . . ? C2 C1 O4 C5 -177.81(17) . . . . ? O2 C4 O5 C6 -1.4(3) . . . . ? C3 C4 O5 C6 179.64(16) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.759 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.072 # Attachment 'Compound_8.CIF' data_p21c _database_code_depnum_ccdc_archive 'CCDC 723069' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H8 Cl8 Nb2 O5' _chemical_formula_weight 617.53 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' 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 8.8939(8) _cell_length_b 15.2128(13) _cell_length_c 13.6512(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.3290(10) _cell_angle_gamma 90.00 _cell_volume 1789.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9929 _cell_measurement_theta_min 2.3635 _cell_measurement_theta_max 28.4465 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 2.483 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5757 _exptl_absorpt_correction_T_max 0.7225 _exptl_absorpt_process_details 'SADABS (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14419 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3905 _reflns_number_gt 3822 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0146P)^2^+1.6234P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3905 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_gt 0.0203 _refine_ls_wR_factor_ref 0.0481 _refine_ls_wR_factor_gt 0.0477 _refine_ls_goodness_of_fit_ref 1.263 _refine_ls_restrained_S_all 1.263 _refine_ls_shift/su_max 0.002 _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 C1 C 0.6245(3) 0.38065(18) 0.7380(2) 0.0275(5) Uani 1 1 d . . . H1A H 0.6350 0.3576 0.8065 0.041 Uiso 1 1 calc R . . H1B H 0.7275 0.3859 0.7247 0.041 Uiso 1 1 calc R . . H1C H 0.5607 0.3404 0.6888 0.041 Uiso 1 1 calc R . . C2 C 0.4339(2) 0.47841(15) 0.76898(16) 0.0162(4) Uani 1 1 d . . . C3 C 0.3672(3) 0.56852(15) 0.75007(17) 0.0195(5) Uani 1 1 d . . . H3A H 0.3001 0.5707 0.6804 0.023 Uiso 1 1 calc R . . H3B H 0.4533 0.6106 0.7536 0.023 Uiso 1 1 calc R . . C4 C 0.2740(3) 0.59870(14) 0.82166(16) 0.0159(4) Uani 1 1 d . . . C5 C 0.1788(3) 0.71929(15) 0.89643(18) 0.0220(5) Uani 1 1 d . . . H5A H 0.0697 0.7038 0.8682 0.033 Uiso 1 1 calc R . . H5B H 0.1894 0.7834 0.9000 0.033 Uiso 1 1 calc R . . H5C H 0.2140 0.6944 0.9645 0.033 Uiso 1 1 calc R . . Cl1 Cl 0.49649(6) 0.18573(4) 0.93389(4) 0.02222(12) Uani 1 1 d . . . Cl2 Cl 0.18899(6) 0.11955(4) 0.75848(4) 0.01895(11) Uani 1 1 d . . . Cl5 Cl 0.27518(7) 0.01530(4) 0.98337(4) 0.02496(13) Uani 1 1 d . . . Cl3 Cl -0.03288(6) 0.15971(4) 0.91510(5) 0.02346(12) Uani 1 1 d . . . Cl4 Cl 0.27223(7) 0.21598(4) 1.08893(4) 0.02081(12) Uani 1 1 d . . . Cl8 Cl 0.05012(6) 0.42038(3) 0.70226(4) 0.01693(11) Uani 1 1 d . . . Cl7 Cl 0.35136(7) 0.43021(4) 1.02968(4) 0.02119(12) Uani 1 1 d . . . Cl6 Cl -0.04183(6) 0.41331(4) 0.92687(4) 0.02059(11) Uani 1 1 d . . . Nb1 Nb 0.23491(2) 0.157157(12) 0.927727(14) 0.01290(5) Uani 1 1 d . . . Nb2 Nb 0.18002(2) 0.403063(12) 0.872425(14) 0.01172(5) Uani 1 1 d . . . O1 O 0.20168(17) 0.28816(10) 0.87704(11) 0.0151(3) Uani 1 1 d . . . O2 O 0.38435(17) 0.41900(10) 0.81443(11) 0.0156(3) Uani 1 1 d . . . O3 O 0.20158(17) 0.54950(10) 0.86508(11) 0.0158(3) Uani 1 1 d . . . O4 O 0.55054(18) 0.46720(11) 0.72936(12) 0.0206(3) Uani 1 1 d . . . O5 O 0.27338(18) 0.68377(10) 0.83152(12) 0.0185(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0176(11) 0.0315(14) 0.0343(14) -0.0058(11) 0.0079(10) 0.0036(10) C2 0.0157(10) 0.0202(11) 0.0119(10) -0.0037(8) 0.0021(8) -0.0036(8) C3 0.0256(12) 0.0190(11) 0.0156(11) 0.0031(8) 0.0082(9) 0.0000(9) C4 0.0164(10) 0.0161(10) 0.0129(10) 0.0007(8) -0.0008(8) -0.0012(8) C5 0.0239(12) 0.0146(11) 0.0282(12) -0.0037(9) 0.0077(10) -0.0014(9) Cl1 0.0148(2) 0.0269(3) 0.0244(3) -0.0053(2) 0.0039(2) 0.0002(2) Cl2 0.0247(3) 0.0174(3) 0.0131(2) -0.00097(19) 0.0015(2) 0.0018(2) Cl5 0.0371(3) 0.0144(3) 0.0204(3) 0.0053(2) 0.0014(2) 0.0022(2) Cl3 0.0170(3) 0.0241(3) 0.0299(3) -0.0015(2) 0.0071(2) -0.0042(2) Cl4 0.0292(3) 0.0210(3) 0.0126(2) -0.00071(19) 0.0057(2) -0.0009(2) Cl8 0.0173(2) 0.0174(2) 0.0146(2) -0.00003(18) 0.00106(19) 0.00032(19) Cl7 0.0243(3) 0.0217(3) 0.0149(2) -0.0011(2) -0.0002(2) -0.0072(2) Cl6 0.0199(3) 0.0215(3) 0.0235(3) -0.0058(2) 0.0114(2) -0.0039(2) Nb1 0.01473(10) 0.01135(10) 0.01190(10) 0.00095(6) 0.00192(7) 0.00019(7) Nb2 0.01317(10) 0.00969(10) 0.01237(10) -0.00092(6) 0.00330(7) -0.00133(6) O1 0.0166(7) 0.0128(7) 0.0152(7) 0.0001(6) 0.0027(6) -0.0005(6) O2 0.0145(7) 0.0145(7) 0.0178(8) -0.0007(6) 0.0039(6) -0.0002(6) O3 0.0175(7) 0.0125(7) 0.0183(8) -0.0010(6) 0.0063(6) -0.0021(6) O4 0.0177(8) 0.0243(9) 0.0225(8) -0.0036(7) 0.0098(6) -0.0023(6) O5 0.0234(8) 0.0120(7) 0.0202(8) 0.0013(6) 0.0056(6) -0.0021(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 C1 O4 1.464(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O2 1.237(3) . ? C2 O4 1.295(3) . ? C2 C3 1.491(3) . ? C3 C4 1.501(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.231(3) . ? C4 O5 1.301(3) . ? C5 O5 1.468(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? Cl1 Nb1 2.3477(6) . ? Cl2 Nb1 2.3163(6) . ? Cl5 Nb1 2.2865(6) . ? Cl3 Nb1 2.3453(6) . ? Cl4 Nb1 2.3221(6) . ? Cl8 Nb2 2.3392(6) . ? Cl7 Nb2 2.3413(6) . ? Cl6 Nb2 2.2794(6) . ? Nb1 O1 2.1063(15) . ? Nb2 O1 1.7581(15) . ? Nb2 O2 2.1680(15) . ? Nb2 O3 2.2404(15) . ? 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 C1 H1A 109.5 . . ? O4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C2 O4 122.3(2) . . ? O2 C2 C3 125.6(2) . . ? O4 C2 C3 111.99(19) . . ? C2 C3 C4 115.38(18) . . ? C2 C3 H3A 108.4 . . ? C4 C3 H3A 108.4 . . ? C2 C3 H3B 108.4 . . ? C4 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? O3 C4 O5 122.6(2) . . ? O3 C4 C3 124.5(2) . . ? O5 C4 C3 112.85(19) . . ? O5 C5 H5A 109.5 . . ? O5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O5 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O1 Nb1 Cl5 179.08(4) . . ? O1 Nb1 Cl2 86.00(4) . . ? Cl5 Nb1 Cl2 94.17(2) . . ? O1 Nb1 Cl4 85.54(4) . . ? Cl5 Nb1 Cl4 94.30(2) . . ? Cl2 Nb1 Cl4 171.51(2) . . ? O1 Nb1 Cl3 84.42(4) . . ? Cl5 Nb1 Cl3 96.48(2) . . ? Cl2 Nb1 Cl3 90.32(2) . . ? Cl4 Nb1 Cl3 88.15(2) . . ? O1 Nb1 Cl1 83.90(4) . . ? Cl5 Nb1 Cl1 95.19(2) . . ? Cl2 Nb1 Cl1 90.57(2) . . ? Cl4 Nb1 Cl1 89.24(2) . . ? Cl3 Nb1 Cl1 168.20(2) . . ? O1 Nb2 O2 91.72(6) . . ? O1 Nb2 O3 168.66(6) . . ? O2 Nb2 O3 77.51(6) . . ? O1 Nb2 Cl6 98.76(5) . . ? O2 Nb2 Cl6 169.38(4) . . ? O3 Nb2 Cl6 92.13(4) . . ? O1 Nb2 Cl8 99.81(5) . . ? O2 Nb2 Cl8 82.96(4) . . ? O3 Nb2 Cl8 82.55(4) . . ? Cl6 Nb2 Cl8 93.52(2) . . ? O1 Nb2 Cl7 95.84(5) . . ? O2 Nb2 Cl7 84.31(4) . . ? O3 Nb2 Cl7 79.75(4) . . ? Cl6 Nb2 Cl7 96.23(2) . . ? Cl8 Nb2 Cl7 160.06(2) . . ? Nb2 O1 Nb1 163.29(9) . . ? C2 O2 Nb2 134.38(15) . . ? C4 O3 Nb2 133.39(14) . . ? C2 O4 C1 118.39(19) . . ? C4 O5 C5 116.49(18) . . ? 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 O2 C2 C3 C4 23.1(3) . . . . ? O4 C2 C3 C4 -158.70(19) . . . . ? C2 C3 C4 O3 -28.8(3) . . . . ? C2 C3 C4 O5 153.01(19) . . . . ? O2 Nb2 O1 Nb1 118.0(3) . . . . ? O3 Nb2 O1 Nb1 100.0(4) . . . . ? Cl6 Nb2 O1 Nb1 -63.7(3) . . . . ? Cl8 Nb2 O1 Nb1 -158.8(3) . . . . ? Cl7 Nb2 O1 Nb1 33.5(3) . . . . ? Cl5 Nb1 O1 Nb2 -84(3) . . . . ? Cl2 Nb1 O1 Nb2 175.4(3) . . . . ? Cl4 Nb1 O1 Nb2 -3.8(3) . . . . ? Cl3 Nb1 O1 Nb2 84.7(3) . . . . ? Cl1 Nb1 O1 Nb2 -93.6(3) . . . . ? O4 C2 O2 Nb2 -169.96(14) . . . . ? C3 C2 O2 Nb2 8.1(3) . . . . ? O1 Nb2 O2 C2 160.6(2) . . . . ? O3 Nb2 O2 C2 -22.97(19) . . . . ? Cl6 Nb2 O2 C2 -10.2(4) . . . . ? Cl8 Nb2 O2 C2 60.92(19) . . . . ? Cl7 Nb2 O2 C2 -103.70(19) . . . . ? O5 C4 O3 Nb2 -177.38(14) . . . . ? C3 C4 O3 Nb2 4.6(3) . . . . ? O1 Nb2 O3 C4 34.7(4) . . . . ? O2 Nb2 O3 C4 16.31(19) . . . . ? Cl6 Nb2 O3 C4 -161.36(19) . . . . ? Cl8 Nb2 O3 C4 -68.08(19) . . . . ? Cl7 Nb2 O3 C4 102.70(19) . . . . ? O2 C2 O4 C1 0.7(3) . . . . ? C3 C2 O4 C1 -177.55(19) . . . . ? O3 C4 O5 C5 -1.1(3) . . . . ? C3 C4 O5 C5 177.15(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.377 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.105