# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Guido Pampaloni' 'Fabio Marchetti' 'Stefano Zacchini' _publ_contact_author_name 'Prof Guido Pampaloni' _publ_contact_author_email PAMPA@DCCI.UNIPI.IT _publ_section_title ; Unusual Room Temperature Activation of 1,2-Dialkoxyalkanes by Niobium and Tantalum Pentachlorides ; # Attachment 'DiglymeHNbCl6.CIF' data_c2c _database_code_depnum_ccdc_archive 'CCDC 691886' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H15 Cl6 Nb O3' _chemical_formula_weight 440.79 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.528(3) _cell_length_b 15.3879(19) _cell_length_c 17.492(2) _cell_angle_alpha 90.00 _cell_angle_beta 124.665(2) _cell_angle_gamma 90.00 _cell_volume 4766.1(10) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4608 _cell_measurement_theta_min 2.633 _cell_measurement_theta_max 28.307 _exptl_crystal_description prism _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2616 _exptl_absorpt_coefficient_mu 1.756 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6987 _exptl_absorpt_correction_T_max 0.7786 _exptl_absorpt_process_details ? _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 11126 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4066 _reflns_number_gt 3464 _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^)+(0.0136P)^2^+6.8882P] 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 4066 _refine_ls_number_parameters 228 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0506 _refine_ls_wR_factor_gt 0.0474 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.181831(14) 0.536602(17) 0.013742(18) 0.01666(7) Uani 1 1 d . . . Cl1 Cl 0.27879(4) 0.54138(5) 0.17261(5) 0.02633(18) Uani 1 1 d . . . Cl2 Cl 0.26212(4) 0.59446(5) -0.02248(5) 0.02767(18) Uani 1 1 d . . . Cl3 Cl 0.21965(4) 0.39303(5) 0.00787(6) 0.03057(19) Uani 1 1 d . . . Cl4 Cl 0.08506(4) 0.52462(5) -0.14509(5) 0.02893(19) Uani 1 1 d . . . Cl5 Cl 0.09949(4) 0.47960(5) 0.04928(6) 0.03162(19) Uani 1 1 d . . . Cl6 Cl 0.14244(4) 0.67641(5) 0.01949(5) 0.02512(17) Uani 1 1 d . . . Nb2 Nb 0.5000 0.5000 1.0000 0.01531(9) Uani 1 2 d S . . Cl7 Cl 0.47644(4) 0.64099(5) 1.02901(5) 0.02505(17) Uani 1 1 d . . . Cl8 Cl 0.53360(4) 0.45582(5) 1.14780(5) 0.02266(17) Uani 1 1 d . . . Cl9 Cl 0.37386(4) 0.46243(5) 0.93605(5) 0.02708(18) Uani 1 1 d . . . C1 C 0.21114(17) 0.84182(19) 0.2094(2) 0.0289(8) Uani 1 1 d . . . H1A H 0.1565 0.8327 0.1755 0.043 Uiso 1 1 calc R . . H1B H 0.2226 0.8689 0.1681 0.043 Uiso 1 1 calc R . . H1C H 0.2282 0.8799 0.2628 0.043 Uiso 1 1 calc R . . O1 O 0.24958(11) 0.75909(13) 0.24169(14) 0.0228(5) Uani 1 1 d . . . C2 C 0.24125(16) 0.7128(2) 0.3081(2) 0.0252(7) Uani 1 1 d . . . H2A H 0.2366 0.7554 0.3469 0.030 Uiso 1 1 calc R . . H2B H 0.2870 0.6775 0.3496 0.030 Uiso 1 1 calc R . . C3 C 0.17344(16) 0.6550(2) 0.2602(2) 0.0259(7) Uani 1 1 d . . . H3A H 0.1741 0.6177 0.2145 0.031 Uiso 1 1 calc R . . H3B H 0.1741 0.6168 0.3063 0.031 Uiso 1 1 calc R . . O2 O 0.10703(11) 0.70696(13) 0.21414(14) 0.0231(5) Uani 1 1 d . . . C4 C 0.04092(17) 0.6566(2) 0.1551(2) 0.0291(8) Uani 1 1 d . . . H4A H 0.0342 0.6142 0.1925 0.035 Uiso 1 1 calc R . . H4B H 0.0456 0.6240 0.1098 0.035 Uiso 1 1 calc R . . C5 C -0.02551(17) 0.7160(2) 0.1050(2) 0.0270(7) Uani 1 1 d . . . H5A H -0.0141 0.7653 0.0785 0.032 Uiso 1 1 calc R . . H5B H -0.0695 0.6843 0.0532 0.032 Uiso 1 1 calc R . . O3 O -0.04374(12) 0.74871(15) 0.16743(14) 0.0306(5) Uani 1 1 d D . . H3 H -0.010(4) 0.752(3) 0.2251(13) 0.037 Uiso 0.50 1 d PD A -1 C6 C -0.10592(16) 0.8095(2) 0.1267(2) 0.0265(7) Uani 1 1 d . . . H6A H -0.0967 0.8569 0.0969 0.040 Uiso 1 1 calc R . . H6B H -0.1104 0.8333 0.1754 0.040 Uiso 1 1 calc R . . H6C H -0.1529 0.7796 0.0801 0.040 Uiso 1 1 calc R . . O4 O 0.5000 0.72197(17) 0.2500 0.0206(6) Uani 1 2 d S . . C7 C 0.43309(15) 0.67124(18) 0.2090(2) 0.0189(6) Uani 1 1 d . . . H7A H 0.4390 0.6264 0.2533 0.023 Uiso 1 1 calc R . . H7B H 0.4226 0.6417 0.1525 0.023 Uiso 1 1 calc R . . C8 C 0.36953(15) 0.73152(19) 0.18446(19) 0.0198(7) Uani 1 1 d . . . H8A H 0.3735 0.7852 0.1562 0.024 Uiso 1 1 calc R . . H8B H 0.3207 0.7033 0.1383 0.024 Uiso 1 1 calc R . . O5 O 0.37217(11) 0.75362(13) 0.26743(14) 0.0212(5) Uani 1 1 d D . . H5 H 0.3295(9) 0.7552(19) 0.260(2) 0.025 Uiso 1 1 d D . . C9 C 0.42160(18) 0.8248(2) 0.3237(2) 0.0325(8) Uani 1 1 d . . . H9A H 0.4737 0.8107 0.3459 0.049 Uiso 1 1 calc R . . H9B H 0.4187 0.8338 0.3771 0.049 Uiso 1 1 calc R . . H9C H 0.4058 0.8779 0.2862 0.049 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 0.01447(14) 0.01695(15) 0.01532(14) 0.00128(12) 0.00655(12) 0.00102(11) Cl1 0.0231(4) 0.0280(4) 0.0167(4) 0.0039(3) 0.0047(3) -0.0021(3) Cl2 0.0250(4) 0.0354(5) 0.0277(4) -0.0003(4) 0.0180(4) -0.0026(3) Cl3 0.0260(4) 0.0213(4) 0.0347(5) -0.0001(4) 0.0115(4) 0.0064(3) Cl4 0.0236(4) 0.0302(5) 0.0172(4) -0.0008(3) 0.0022(3) -0.0004(3) Cl5 0.0331(4) 0.0322(5) 0.0377(5) -0.0062(4) 0.0250(4) -0.0115(4) Cl6 0.0257(4) 0.0211(4) 0.0251(4) -0.0007(3) 0.0124(4) 0.0045(3) Nb2 0.01538(19) 0.0141(2) 0.0151(2) -0.00099(16) 0.00789(17) -0.00001(15) Cl7 0.0350(4) 0.0174(4) 0.0256(4) 0.0000(3) 0.0189(4) 0.0048(3) Cl8 0.0269(4) 0.0225(4) 0.0177(4) 0.0006(3) 0.0122(3) -0.0004(3) Cl9 0.0170(4) 0.0313(5) 0.0288(4) -0.0012(4) 0.0106(4) -0.0038(3) C1 0.0266(17) 0.0241(18) 0.036(2) 0.0046(15) 0.0178(16) 0.0067(14) O1 0.0221(11) 0.0243(12) 0.0273(12) 0.0045(10) 0.0173(10) 0.0064(9) C2 0.0223(16) 0.0341(19) 0.0200(17) 0.0088(15) 0.0126(15) 0.0099(14) C3 0.0282(18) 0.0252(18) 0.0326(19) 0.0071(15) 0.0222(16) 0.0057(14) O2 0.0174(11) 0.0254(12) 0.0266(12) -0.0028(10) 0.0126(10) 0.0015(9) C4 0.0266(18) 0.0281(19) 0.037(2) -0.0099(16) 0.0206(17) -0.0076(15) C5 0.0247(17) 0.034(2) 0.0236(18) -0.0077(15) 0.0149(15) -0.0064(15) O3 0.0237(13) 0.0479(15) 0.0216(12) 0.0093(11) 0.0139(11) 0.0156(11) C6 0.0185(16) 0.0292(19) 0.0293(19) 0.0068(15) 0.0121(15) 0.0044(14) O4 0.0147(14) 0.0185(16) 0.0287(17) 0.000 0.0124(14) 0.000 C7 0.0175(15) 0.0184(16) 0.0226(17) -0.0037(13) 0.0125(14) -0.0054(12) C8 0.0173(15) 0.0251(18) 0.0166(16) 0.0015(13) 0.0094(14) 0.0000(13) O5 0.0153(10) 0.0266(12) 0.0247(12) -0.0030(9) 0.0132(10) 0.0000(9) C9 0.0303(19) 0.032(2) 0.032(2) -0.0107(16) 0.0163(17) -0.0034(15) _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 Cl2 2.3297(8) . ? Nb1 Cl6 2.3355(8) . ? Nb1 Cl1 2.3423(8) . ? Nb1 Cl4 2.3471(8) . ? Nb1 Cl5 2.3561(8) . ? Nb1 Cl3 2.3769(8) . ? Nb2 Cl9 2.3461(8) 5_667 ? Nb2 Cl9 2.3462(8) . ? Nb2 Cl7 2.3483(8) . ? Nb2 Cl7 2.3483(7) 5_667 ? Nb2 Cl8 2.3542(7) 5_667 ? Nb2 Cl8 2.3542(7) . ? C1 O1 1.447(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O1 C2 1.457(3) . ? C2 C3 1.495(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O2 1.422(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O2 C4 1.422(3) . ? C4 C5 1.491(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 O3 1.444(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? O3 C6 1.446(3) . ? O3 H3 0.845(10) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O4 C7 1.423(3) . ? O4 C7 1.423(3) 2_655 ? C7 C8 1.499(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O5 1.460(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? O5 C9 1.453(3) . ? O5 H5 0.853(10) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 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 Cl2 Nb1 Cl6 90.19(3) . . ? Cl2 Nb1 Cl1 90.71(3) . . ? Cl6 Nb1 Cl1 91.17(3) . . ? Cl2 Nb1 Cl4 90.25(3) . . ? Cl6 Nb1 Cl4 91.36(3) . . ? Cl1 Nb1 Cl4 177.29(3) . . ? Cl2 Nb1 Cl5 179.24(3) . . ? Cl6 Nb1 Cl5 89.17(3) . . ? Cl1 Nb1 Cl5 89.72(3) . . ? Cl4 Nb1 Cl5 89.35(3) . . ? Cl2 Nb1 Cl3 91.04(3) . . ? Cl6 Nb1 Cl3 178.73(3) . . ? Cl1 Nb1 Cl3 89.11(3) . . ? Cl4 Nb1 Cl3 88.34(3) . . ? Cl5 Nb1 Cl3 89.60(3) . . ? Cl9 Nb2 Cl9 180.0 5_667 . ? Cl9 Nb2 Cl7 90.17(3) 5_667 . ? Cl9 Nb2 Cl7 89.83(3) . . ? Cl9 Nb2 Cl7 89.83(3) 5_667 5_667 ? Cl9 Nb2 Cl7 90.17(3) . 5_667 ? Cl7 Nb2 Cl7 180.000(1) . 5_667 ? Cl9 Nb2 Cl8 90.10(3) 5_667 5_667 ? Cl9 Nb2 Cl8 89.90(3) . 5_667 ? Cl7 Nb2 Cl8 90.07(3) . 5_667 ? Cl7 Nb2 Cl8 89.93(3) 5_667 5_667 ? Cl9 Nb2 Cl8 89.90(3) 5_667 . ? Cl9 Nb2 Cl8 90.10(3) . . ? Cl7 Nb2 Cl8 89.93(3) . . ? Cl7 Nb2 Cl8 90.07(3) 5_667 . ? Cl8 Nb2 Cl8 180.000(16) 5_667 . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 O1 C2 116.0(2) . . ? O1 C2 C3 111.6(2) . . ? O1 C2 H2A 109.3 . . ? C3 C2 H2A 109.3 . . ? O1 C2 H2B 109.3 . . ? C3 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? O2 C3 C2 109.2(2) . . ? O2 C3 H3A 109.8 . . ? C2 C3 H3A 109.8 . . ? O2 C3 H3B 109.8 . . ? C2 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? C4 O2 C3 111.9(2) . . ? O2 C4 C5 108.7(2) . . ? O2 C4 H4A 109.9 . . ? C5 C4 H4A 109.9 . . ? O2 C4 H4B 109.9 . . ? C5 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? O3 C5 C4 110.6(2) . . ? O3 C5 H5A 109.5 . . ? C4 C5 H5A 109.5 . . ? O3 C5 H5B 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C5 O3 C6 115.2(2) . . ? C5 O3 H3 121(6) . . ? C6 O3 H3 118(5) . . ? O3 C6 H6A 109.5 . . ? O3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C7 O4 C7 113.4(3) . 2_655 ? O4 C7 C8 107.6(2) . . ? O4 C7 H7A 110.2 . . ? C8 C7 H7A 110.2 . . ? O4 C7 H7B 110.2 . . ? C8 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? O5 C8 C7 110.2(2) . . ? O5 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? O5 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C9 O5 C8 116.7(2) . . ? C9 O5 H5 113(2) . . ? C8 O5 H5 115(2) . . ? O5 C9 H9A 109.5 . . ? O5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 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 C1 O1 C2 C3 89.0(3) . . . . ? O1 C2 C3 O2 -69.5(3) . . . . ? C2 C3 O2 C4 170.5(2) . . . . ? C3 O2 C4 C5 -176.5(2) . . . . ? O2 C4 C5 O3 -72.8(3) . . . . ? C4 C5 O3 C6 178.0(2) . . . . ? C7 O4 C7 C8 169.9(3) 2_655 . . . ? O4 C7 C8 O5 -77.8(3) . . . . ? C7 C8 O5 C9 84.5(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O3 0.845(10) 1.550(16) 2.388(4) 171(8) 2 O5 H5 O1 0.853(10) 1.561(10) 2.413(2) 177(3) . _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.403 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.074 # Attachment 'Nb-O-Nb.CIF' data_p212121 _database_code_depnum_ccdc_archive 'CCDC 691887' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H10 Cl8 Nb2 O3' _chemical_formula_weight 575.54 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 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 7.0287(5) _cell_length_b 13.5297(9) _cell_length_c 17.5555(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1669.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7726 _cell_measurement_theta_min 2.320 _cell_measurement_theta_max 28.6855 _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 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 2.644 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6067 _exptl_absorpt_correction_T_max 0.7421 _exptl_absorpt_process_details ? _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 9274 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3564 _reflns_number_gt 3496 _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^)+(0.0129P)^2^+0.2996P] 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 0.00(3) _refine_ls_number_reflns 3564 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0144 _refine_ls_R_factor_gt 0.0138 _refine_ls_wR_factor_ref 0.0327 _refine_ls_wR_factor_gt 0.0325 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.62536(3) 0.095614(14) 0.162928(9) 0.01085(4) Uani 1 1 d . . . Nb2 Nb 0.50147(3) -0.043362(14) -0.023167(9) 0.01226(5) Uani 1 1 d . . . Cl1 Cl 0.76334(8) 0.02220(4) -0.08677(3) 0.02156(12) Uani 1 1 d . . . Cl2 Cl 0.40627(8) -0.13701(4) -0.12403(3) 0.02091(12) Uani 1 1 d . . . Cl3 Cl 0.32875(8) 0.09778(4) -0.05762(3) 0.02228(12) Uani 1 1 d . . . Cl4 Cl 0.24364(8) -0.08872(4) 0.05269(3) 0.01745(11) Uani 1 1 d . . . Cl5 Cl 0.69029(8) -0.16421(4) 0.03118(3) 0.02129(12) Uani 1 1 d . . . Cl6 Cl 0.45264(7) 0.24004(4) 0.13461(3) 0.01709(11) Uani 1 1 d . . . Cl7 Cl 0.85620(9) -0.01550(4) 0.20671(3) 0.02028(12) Uani 1 1 d . . . Cl8 Cl 0.38388(8) 0.02300(4) 0.23043(3) 0.01978(12) Uani 1 1 d . . . O1 O 0.5906(2) 0.04163(11) 0.07292(8) 0.0149(3) Uani 1 1 d . . . O2 O 0.8701(2) 0.18427(11) 0.13211(8) 0.0131(3) Uani 1 1 d . . . O3 O 0.7071(2) 0.18824(11) 0.26708(8) 0.0139(3) Uani 1 1 d . . . C1 C 0.9965(3) 0.15407(17) 0.07020(11) 0.0189(5) Uani 1 1 d . . . H1A H 1.0671 0.2117 0.0516 0.028 Uiso 1 1 calc R . . H1B H 0.9209 0.1260 0.0286 0.028 Uiso 1 1 calc R . . H1C H 1.0862 0.1042 0.0890 0.028 Uiso 1 1 calc R . . C2 C 0.9736(3) 0.23320(16) 0.19304(11) 0.0147(4) Uani 1 1 d . . . H2A H 1.0503 0.2884 0.1724 0.018 Uiso 1 1 calc R . . H2B H 1.0602 0.1860 0.2186 0.018 Uiso 1 1 calc R . . C3 C 0.8292(3) 0.27122(16) 0.24813(12) 0.0157(5) Uani 1 1 d . . . H3A H 0.8923 0.2970 0.2945 0.019 Uiso 1 1 calc R . . H3B H 0.7539 0.3252 0.2248 0.019 Uiso 1 1 calc R . . C4 C 0.5761(3) 0.21431(18) 0.32779(12) 0.0202(5) Uani 1 1 d . . . H4A H 0.6480 0.2385 0.3718 0.030 Uiso 1 1 calc R . . H4B H 0.5024 0.1559 0.3426 0.030 Uiso 1 1 calc R . . H4C H 0.4895 0.2661 0.3100 0.030 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 0.01224(9) 0.00920(9) 0.01111(8) -0.00090(7) 0.00065(7) -0.00061(8) Nb2 0.01560(10) 0.01023(9) 0.01094(8) 0.00004(7) 0.00086(7) -0.00079(8) Cl1 0.0232(3) 0.0235(3) 0.0180(2) -0.0022(2) 0.0055(2) -0.0087(3) Cl2 0.0231(3) 0.0232(3) 0.0164(2) -0.0059(2) 0.0006(2) -0.0061(2) Cl3 0.0271(3) 0.0174(3) 0.0224(2) 0.0076(2) 0.0020(2) 0.0053(3) Cl4 0.0186(3) 0.0147(3) 0.0190(2) 0.0013(2) 0.0042(2) -0.0018(2) Cl5 0.0256(3) 0.0171(3) 0.0211(2) 0.0010(2) -0.0003(2) 0.0071(2) Cl6 0.0133(3) 0.0144(3) 0.0235(2) 0.0012(2) -0.0020(2) 0.0021(2) Cl7 0.0244(3) 0.0153(3) 0.0211(2) 0.0020(2) -0.0014(2) 0.0060(3) Cl8 0.0225(3) 0.0178(3) 0.0190(2) -0.0010(2) 0.0063(2) -0.0063(3) O1 0.0177(8) 0.0144(8) 0.0126(6) -0.0009(6) 0.0024(6) -0.0031(7) O2 0.0120(7) 0.0136(8) 0.0137(6) -0.0019(5) 0.0018(6) -0.0010(7) O3 0.0147(8) 0.0136(8) 0.0134(6) -0.0028(6) 0.0019(6) -0.0017(6) C1 0.0158(11) 0.0238(12) 0.0170(9) -0.0045(8) 0.0048(9) -0.0006(11) C2 0.0142(11) 0.0150(11) 0.0149(9) -0.0008(8) -0.0021(8) -0.0020(10) C3 0.0157(11) 0.0123(11) 0.0192(10) -0.0011(8) 0.0008(8) -0.0039(9) C4 0.0213(12) 0.0237(13) 0.0155(10) -0.0058(9) 0.0061(9) -0.0010(10) _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 1.7579(14) . ? Nb1 O2 2.1661(15) . ? Nb1 O3 2.2898(14) . ? Nb1 Cl8 2.2913(6) . ? Nb1 Cl7 2.3417(6) . ? Nb1 Cl6 2.3536(6) . ? Nb2 O1 2.1353(14) . ? Nb2 Cl2 2.2778(6) . ? Nb2 Cl5 2.3120(6) . ? Nb2 Cl1 2.3284(6) . ? Nb2 Cl4 2.3311(6) . ? Nb2 Cl3 2.3423(6) . ? O2 C2 1.453(2) . ? O2 C1 1.462(2) . ? O3 C3 1.452(3) . ? O3 C4 1.452(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.493(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 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 O2 96.67(6) . . ? O1 Nb1 O3 168.53(6) . . ? O2 Nb1 O3 72.37(5) . . ? O1 Nb1 Cl8 100.58(5) . . ? O2 Nb1 Cl8 162.75(4) . . ? O3 Nb1 Cl8 90.43(4) . . ? O1 Nb1 Cl7 97.17(5) . . ? O2 Nb1 Cl7 83.52(4) . . ? O3 Nb1 Cl7 85.15(4) . . ? Cl8 Nb1 Cl7 93.91(2) . . ? O1 Nb1 Cl6 94.78(5) . . ? O2 Nb1 Cl6 84.10(4) . . ? O3 Nb1 Cl6 81.01(4) . . ? Cl8 Nb1 Cl6 94.77(2) . . ? Cl7 Nb1 Cl6 163.69(2) . . ? O1 Nb2 Cl2 178.76(4) . . ? O1 Nb2 Cl5 83.48(4) . . ? Cl2 Nb2 Cl5 95.51(2) . . ? O1 Nb2 Cl1 86.67(4) . . ? Cl2 Nb2 Cl1 94.09(2) . . ? Cl5 Nb2 Cl1 90.78(2) . . ? O1 Nb2 Cl4 85.32(4) . . ? Cl2 Nb2 Cl4 93.97(2) . . ? Cl5 Nb2 Cl4 91.39(2) . . ? Cl1 Nb2 Cl4 171.41(2) . . ? O1 Nb2 Cl3 85.23(4) . . ? Cl2 Nb2 Cl3 95.77(2) . . ? Cl5 Nb2 Cl3 168.71(2) . . ? Cl1 Nb2 Cl3 88.58(2) . . ? Cl4 Nb2 Cl3 87.66(2) . . ? Nb1 O1 Nb2 167.07(9) . . ? C2 O2 C1 111.77(16) . . ? C2 O2 Nb1 117.76(11) . . ? C1 O2 Nb1 120.90(12) . . ? C3 O3 C4 110.80(16) . . ? C3 O3 Nb1 112.86(11) . . ? C4 O3 Nb1 124.07(13) . . ? 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 107.09(17) . . ? 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 C2 106.48(17) . . ? O3 C3 H3A 110.4 . . ? C2 C3 H3A 110.4 . . ? O3 C3 H3B 110.4 . . ? C2 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? O3 C4 H4A 109.5 . . ? O3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 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 O2 Nb1 O1 Nb2 173.0(4) . . . . ? O3 Nb1 O1 Nb2 -170.2(2) . . . . ? Cl8 Nb1 O1 Nb2 -6.6(4) . . . . ? Cl7 Nb1 O1 Nb2 88.7(4) . . . . ? Cl6 Nb1 O1 Nb2 -102.4(4) . . . . ? Cl2 Nb2 O1 Nb1 -42(2) . . . . ? Cl5 Nb2 O1 Nb1 -77.9(4) . . . . ? Cl1 Nb2 O1 Nb1 -169.1(4) . . . . ? Cl4 Nb2 O1 Nb1 14.0(4) . . . . ? Cl3 Nb2 O1 Nb1 102.0(4) . . . . ? O1 Nb1 O2 C2 -170.44(14) . . . . ? O3 Nb1 O2 C2 13.01(13) . . . . ? Cl8 Nb1 O2 C2 8.3(2) . . . . ? Cl7 Nb1 O2 C2 -73.94(14) . . . . ? Cl6 Nb1 O2 C2 95.42(14) . . . . ? O1 Nb1 O2 C1 -26.98(15) . . . . ? O3 Nb1 O2 C1 156.46(15) . . . . ? Cl8 Nb1 O2 C1 151.79(13) . . . . ? Cl7 Nb1 O2 C1 69.51(14) . . . . ? Cl6 Nb1 O2 C1 -121.12(14) . . . . ? O1 Nb1 O3 C3 0.0(4) . . . . ? O2 Nb1 O3 C3 17.53(13) . . . . ? Cl8 Nb1 O3 C3 -163.85(13) . . . . ? Cl7 Nb1 O3 C3 102.26(13) . . . . ? Cl6 Nb1 O3 C3 -69.09(13) . . . . ? O1 Nb1 O3 C4 138.7(3) . . . . ? O2 Nb1 O3 C4 156.15(16) . . . . ? Cl8 Nb1 O3 C4 -25.23(15) . . . . ? Cl7 Nb1 O3 C4 -119.12(15) . . . . ? Cl6 Nb1 O3 C4 69.53(15) . . . . ? C1 O2 C2 C3 173.36(17) . . . . ? Nb1 O2 C2 C3 -40.0(2) . . . . ? C4 O3 C3 C2 172.79(16) . . . . ? Nb1 O3 C3 C2 -43.07(19) . . . . ? O2 C2 C3 O3 52.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.255 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.061 # Attachment 'Ta-O-Ta.CIF' data_p21n _database_code_depnum_ccdc_archive 'CCDC 691888' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H10 Cl8 O3 Ta2' _chemical_formula_weight 751.62 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' Ta Ta -0.7052 6.5227 '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 6.6388(3) _cell_length_b 26.0083(13) _cell_length_c 9.9726(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.1160(10) _cell_angle_gamma 90.00 _cell_volume 1676.99(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8234 _cell_measurement_theta_min 2.6175 _cell_measurement_theta_max 28.400 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.977 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 14.305 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2080 _exptl_absorpt_correction_T_max 0.2786 _exptl_absorpt_process_details ? _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 18476 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3666 _reflns_number_gt 3236 _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^)+(0.0194P)^2^+0.7379P] 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 3666 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0428 _refine_ls_wR_factor_gt 0.0411 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta2 Ta 0.72695(2) 0.107556(6) 0.165119(17) 0.01561(5) Uani 1 1 d . . . Cl1 Cl 0.57609(16) 0.03196(4) 0.22393(11) 0.0240(2) Uani 1 1 d . . . Cl2 Cl 0.57595(16) 0.09725(4) -0.06780(11) 0.0233(2) Uani 1 1 d . . . Cl3 Cl 1.01998(15) 0.05976(4) 0.14619(11) 0.0198(2) Uani 1 1 d . . . Cl4 Cl 0.89807(15) 0.18221(4) 0.12311(10) 0.0199(2) Uani 1 1 d . . . Cl5 Cl 0.45258(16) 0.15602(4) 0.20433(11) 0.0247(2) Uani 1 1 d . . . O1 O 0.8639(4) 0.11745(10) 0.3671(3) 0.0186(6) Uani 1 1 d . . . Ta1 Ta 1.01246(2) 0.141954(6) 0.528270(17) 0.01516(5) Uani 1 1 d . . . Cl6 Cl 1.29119(15) 0.08540(4) 0.54271(11) 0.0225(2) Uani 1 1 d . . . Cl7 Cl 0.74776(16) 0.19338(4) 0.57423(11) 0.0247(2) Uani 1 1 d . . . Cl8 Cl 1.18057(16) 0.20829(4) 0.45432(11) 0.0220(2) Uani 1 1 d . . . O2 O 0.9037(4) 0.08434(10) 0.6507(3) 0.0176(6) Uani 1 1 d . . . O3 O 1.1598(4) 0.15842(10) 0.7484(3) 0.0189(6) Uani 1 1 d . . . C1 C 0.8150(7) 0.03515(16) 0.5945(5) 0.0250(10) Uani 1 1 d . . . H1A H 0.9262 0.0101 0.5980 0.038 Uiso 1 1 calc R . . H1B H 0.7397 0.0400 0.4987 0.038 Uiso 1 1 calc R . . H1C H 0.7197 0.0226 0.6491 0.038 Uiso 1 1 calc R . . C2 C 1.0170(6) 0.07897(16) 0.7939(4) 0.0203(9) Uani 1 1 d . . . H2A H 1.1475 0.0598 0.7994 0.024 Uiso 1 1 calc R . . H2B H 0.9325 0.0603 0.8482 0.024 Uiso 1 1 calc R . . C3 C 1.0606(7) 0.13250(16) 0.8469(4) 0.0213(9) Uani 1 1 d . . . H3A H 0.9307 0.1502 0.8523 0.026 Uiso 1 1 calc R . . H3B H 1.1537 0.1321 0.9398 0.026 Uiso 1 1 calc R . . C4 C 1.2405(8) 0.20836(17) 0.8016(5) 0.0357(12) Uani 1 1 d . . . H4A H 1.1263 0.2330 0.7916 0.054 Uiso 1 1 calc R . . H4B H 1.3401 0.2206 0.7498 0.054 Uiso 1 1 calc R . . H4C H 1.3092 0.2051 0.8991 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 Ta2 0.01659(9) 0.01539(9) 0.01401(9) -0.00069(6) 0.00171(6) 0.00048(6) Cl1 0.0240(5) 0.0220(5) 0.0257(6) -0.0001(4) 0.0051(4) -0.0058(4) Cl2 0.0223(5) 0.0282(5) 0.0172(5) -0.0036(4) -0.0002(4) 0.0017(4) Cl3 0.0206(5) 0.0179(5) 0.0209(5) 0.0018(4) 0.0047(4) 0.0034(4) Cl4 0.0264(5) 0.0152(5) 0.0184(5) 0.0012(4) 0.0054(4) 0.0004(4) Cl5 0.0205(5) 0.0294(5) 0.0235(6) -0.0044(4) 0.0036(4) 0.0051(4) O1 0.0196(15) 0.0188(14) 0.0169(15) 0.0003(12) 0.0034(12) -0.0018(11) Ta1 0.01759(9) 0.01389(8) 0.01321(9) 0.00005(6) 0.00188(6) -0.00032(6) Cl6 0.0217(5) 0.0211(5) 0.0246(6) -0.0007(4) 0.0051(4) 0.0031(4) Cl7 0.0249(5) 0.0239(5) 0.0252(6) 0.0005(4) 0.0055(4) 0.0072(4) Cl8 0.0259(5) 0.0187(5) 0.0208(5) -0.0001(4) 0.0041(4) -0.0049(4) O2 0.0210(15) 0.0147(14) 0.0163(15) -0.0006(11) 0.0027(12) -0.0019(11) O3 0.0272(16) 0.0160(14) 0.0136(15) 0.0003(11) 0.0048(12) -0.0039(11) C1 0.031(2) 0.017(2) 0.024(2) 0.0003(18) 0.0009(19) -0.0093(17) C2 0.024(2) 0.022(2) 0.015(2) 0.0007(17) 0.0052(17) -0.0017(17) C3 0.028(2) 0.023(2) 0.014(2) 0.0018(17) 0.0067(18) -0.0005(17) C4 0.054(3) 0.019(2) 0.026(3) -0.0044(19) -0.005(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 Ta2 O1 2.030(3) . ? Ta2 Cl5 2.3201(10) . ? Ta2 Cl2 2.3272(10) . ? Ta2 Cl4 2.3348(10) . ? Ta2 Cl1 2.3407(10) . ? Ta2 Cl3 2.3521(10) . ? O1 Ta1 1.800(3) . ? Ta1 O2 2.158(3) . ? Ta1 O3 2.232(3) . ? Ta1 Cl8 2.2671(10) . ? Ta1 Cl7 2.3351(10) . ? Ta1 Cl6 2.3424(10) . ? O2 C2 1.462(5) . ? O2 C1 1.466(5) . ? O3 C4 1.458(5) . ? O3 C3 1.465(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.494(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 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 Ta2 Cl5 87.47(8) . . ? O1 Ta2 Cl2 178.71(8) . . ? Cl5 Ta2 Cl2 93.09(4) . . ? O1 Ta2 Cl4 86.91(8) . . ? Cl5 Ta2 Cl4 90.63(4) . . ? Cl2 Ta2 Cl4 91.93(4) . . ? O1 Ta2 Cl1 88.77(8) . . ? Cl5 Ta2 Cl1 90.99(4) . . ? Cl2 Ta2 Cl1 92.37(4) . . ? Cl4 Ta2 Cl1 175.32(4) . . ? O1 Ta2 Cl3 87.38(8) . . ? Cl5 Ta2 Cl3 174.85(4) . . ? Cl2 Ta2 Cl3 92.05(4) . . ? Cl4 Ta2 Cl3 88.86(3) . . ? Cl1 Ta2 Cl3 89.13(4) . . ? Ta1 O1 Ta2 164.15(16) . . ? O1 Ta1 O2 94.21(11) . . ? O1 Ta1 O3 167.03(11) . . ? O2 Ta1 O3 72.84(10) . . ? O1 Ta1 Cl8 100.92(9) . . ? O2 Ta1 Cl8 164.80(8) . . ? O3 Ta1 Cl8 92.05(7) . . ? O1 Ta1 Cl7 95.38(9) . . ? O2 Ta1 Cl7 85.61(8) . . ? O3 Ta1 Cl7 83.01(8) . . ? Cl8 Ta1 Cl7 94.35(4) . . ? O1 Ta1 Cl6 95.61(9) . . ? O2 Ta1 Cl6 83.70(8) . . ? O3 Ta1 Cl6 84.05(8) . . ? Cl8 Ta1 Cl6 93.30(4) . . ? Cl7 Ta1 Cl6 165.18(4) . . ? C2 O2 C1 111.3(3) . . ? C2 O2 Ta1 117.1(2) . . ? C1 O2 Ta1 123.1(2) . . ? C4 O3 C3 110.5(3) . . ? C4 O3 Ta1 124.9(3) . . ? C3 O3 Ta1 114.1(2) . . ? 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 105.8(3) . . ? O2 C2 H2A 110.6 . . ? C3 C2 H2A 110.6 . . ? O2 C2 H2B 110.6 . . ? C3 C2 H2B 110.6 . . ? H2A C2 H2B 108.7 . . ? O3 C3 C2 105.8(3) . . ? O3 C3 H3A 110.6 . . ? C2 C3 H3A 110.6 . . ? O3 C3 H3B 110.6 . . ? C2 C3 H3B 110.6 . . ? H3A C3 H3B 108.7 . . ? O3 C4 H4A 109.5 . . ? O3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 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 Cl5 Ta2 O1 Ta1 -88.3(6) . . . . ? Cl2 Ta2 O1 Ta1 28(4) . . . . ? Cl4 Ta2 O1 Ta1 2.5(6) . . . . ? Cl1 Ta2 O1 Ta1 -179.3(6) . . . . ? Cl3 Ta2 O1 Ta1 91.5(6) . . . . ? Ta2 O1 Ta1 O2 173.8(6) . . . . ? Ta2 O1 Ta1 O3 170.0(4) . . . . ? Ta2 O1 Ta1 Cl8 -7.7(6) . . . . ? Ta2 O1 Ta1 Cl7 87.8(6) . . . . ? Ta2 O1 Ta1 Cl6 -102.1(6) . . . . ? O1 Ta1 O2 C2 165.8(3) . . . . ? O3 Ta1 O2 C2 -15.1(2) . . . . ? Cl8 Ta1 O2 C2 -8.7(5) . . . . ? Cl7 Ta1 O2 C2 -99.1(2) . . . . ? Cl6 Ta1 O2 C2 70.6(2) . . . . ? O1 Ta1 O2 C1 20.6(3) . . . . ? O3 Ta1 O2 C1 -160.3(3) . . . . ? Cl8 Ta1 O2 C1 -153.9(3) . . . . ? Cl7 Ta1 O2 C1 115.7(3) . . . . ? Cl6 Ta1 O2 C1 -74.6(3) . . . . ? O1 Ta1 O3 C4 -153.4(5) . . . . ? O2 Ta1 O3 C4 -157.3(3) . . . . ? Cl8 Ta1 O3 C4 24.3(3) . . . . ? Cl7 Ta1 O3 C4 -69.8(3) . . . . ? Cl6 Ta1 O3 C4 117.4(3) . . . . ? O1 Ta1 O3 C3 -12.3(6) . . . . ? O2 Ta1 O3 C3 -16.3(2) . . . . ? Cl8 Ta1 O3 C3 165.4(2) . . . . ? Cl7 Ta1 O3 C3 71.3(2) . . . . ? Cl6 Ta1 O3 C3 -101.5(2) . . . . ? C1 O2 C2 C3 -168.6(3) . . . . ? Ta1 O2 C2 C3 42.3(4) . . . . ? C4 O3 C3 C2 -170.6(3) . . . . ? Ta1 O3 C3 C2 42.9(4) . . . . ? O2 C2 C3 O3 -52.5(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.336 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.141