Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Esther C. E. Rosenthal' _publ_contact_author_address ; Institut fur Chemie Technische Universitat Berlin Sekretariat C2 Stra\&se des 17. Juni 135 Berlin 10623 GERMANY ; _publ_contact_author_email esther.rosenthal@tu-berlin.de _publ_contact_author_phone +4930-31429746 _publ_contact_author_fax +4930-31422168 _publ_section_title ; Chloride-bridged oxovanadium(V) complexes with alkoxyalkoxide ligands. Synthesis, structure, electrochemistry and reactivities ; loop_ _publ_author_name E.C.E.Rosenthal M.Hummert S.Dechert H.Cui 'P.Escarpa Gaede' ; J.'Koch ; data_3 _database_code_depnum_ccdc_archive 'CCDC 270039' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H22 Cl4 O6 V2' _chemical_formula_sum 'C10 H22 Cl4 O6 V2' _chemical_formula_weight 481.96 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' V V 0.3005 0.5294 '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 7.2385(2) _cell_length_b 7.3552(1) _cell_length_c 9.4709(2) _cell_angle_alpha 102.775(1) _cell_angle_beta 96.106(1) _cell_angle_gamma 109.218(1) _cell_volume 455.478(17) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5134 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 244 _exptl_absorpt_coefficient_mu 1.633 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.543 _exptl_absorpt_correction_T_max 0.719 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3498 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2056 _reflns_number_gt 1781 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai & Huttner, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0619P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2056 _refine_ls_number_parameters 102 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0985 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 V1 V 0.60005(6) 0.75505(6) 0.63924(4) 0.01623(14) Uani 1 1 d . . . Cl1 Cl 0.61036(8) 0.42086(8) 0.60687(6) 0.01853(15) Uani 1 1 d . . . Cl2 Cl 0.75583(9) 0.82740(10) 0.87655(6) 0.02573(17) Uani 1 1 d . . . O1 O 0.7903(3) 0.8501(3) 0.5739(2) 0.0270(4) Uani 1 1 d . . . O2 O 0.5007(3) 0.9471(3) 0.65307(19) 0.0236(4) Uani 1 1 d . . . O3 O 0.3108(2) 0.6199(3) 0.71322(19) 0.0209(4) Uani 1 1 d . . . C1 C 0.3197(4) 0.9392(4) 0.7054(3) 0.0294(6) Uani 1 1 d . . . H1A H 0.2530 1.0077 0.6540 0.080 Uiso 1 1 calc R . . H1B H 0.3512 1.0072 0.8099 0.080 Uiso 1 1 calc R . . C2 C 0.1829(4) 0.7251(4) 0.6799(3) 0.0263(5) Uani 1 1 d . . . H2A H 0.0864 0.7166 0.7441 0.080 Uiso 1 1 calc R . . H2B H 0.1119 0.6694 0.5782 0.080 Uiso 1 1 calc R . . C3 C 0.2631(4) 0.5012(4) 0.8195(2) 0.0196(5) Uani 1 1 d . . . H3 H 0.3689 0.4476 0.8337 0.080 Uiso 1 1 calc R . . C4 C 0.0687(4) 0.3239(4) 0.7558(3) 0.0254(5) Uani 1 1 d . . . H4A H -0.0400 0.3709 0.7483 0.080 Uiso 1 1 calc R . . H4B H 0.0488 0.2368 0.8194 0.080 Uiso 1 1 calc R . . H4C H 0.0746 0.2520 0.6596 0.080 Uiso 1 1 calc R . . C5 C 0.2639(5) 0.6308(5) 0.9687(3) 0.0335(6) Uani 1 1 d . . . H5A H 0.3834 0.7481 0.9978 0.080 Uiso 1 1 calc R . . H5B H 0.2590 0.5564 1.0406 0.080 Uiso 1 1 calc R . . H5C H 0.1498 0.6698 0.9620 0.080 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 V1 0.0142(2) 0.0165(2) 0.0167(2) 0.00402(15) 0.00269(15) 0.00433(16) Cl1 0.0191(3) 0.0218(3) 0.0170(3) 0.0047(2) 0.0012(2) 0.0115(2) Cl2 0.0224(3) 0.0301(3) 0.0192(3) 0.0020(2) -0.0019(2) 0.0075(3) O1 0.0207(9) 0.0282(10) 0.0276(9) 0.0075(8) 0.0067(7) 0.0027(8) O2 0.0261(9) 0.0189(9) 0.0252(9) 0.0050(7) 0.0029(7) 0.0089(8) O3 0.0187(8) 0.0271(9) 0.0270(9) 0.0155(7) 0.0103(7) 0.0143(7) C1 0.0297(14) 0.0261(14) 0.0399(15) 0.0089(11) 0.0099(12) 0.0188(12) C2 0.0223(12) 0.0352(15) 0.0305(13) 0.0140(11) 0.0081(10) 0.0178(12) C3 0.0180(11) 0.0251(12) 0.0197(11) 0.0117(10) 0.0065(9) 0.0086(10) C4 0.0221(12) 0.0261(13) 0.0276(13) 0.0076(10) 0.0077(10) 0.0074(11) C5 0.0327(15) 0.0405(17) 0.0227(13) 0.0063(12) 0.0070(11) 0.0086(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O1 1.5836(18) . ? V1 O2 1.7713(17) . ? V1 O3 2.2612(17) . ? V1 Cl2 2.2679(7) . ? V1 Cl1 2.4359(6) . ? V1 Cl1 2.4577(6) 2_666 ? Cl1 V1 2.4577(6) 2_666 ? O2 C1 1.437(3) . ? O3 C2 1.440(3) . ? O3 C3 1.469(3) . ? C1 C2 1.508(4) . ? C3 C5 1.518(4) . ? C3 C4 1.519(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 V1 O2 99.28(10) . . ? O1 V1 O3 174.59(8) . . ? O2 V1 O3 78.13(8) . . ? O1 V1 Cl2 97.95(7) . . ? O2 V1 Cl2 100.39(6) . . ? O3 V1 Cl2 87.22(5) . . ? O1 V1 Cl1 98.47(7) . . ? O2 V1 Cl1 159.46(7) . . ? O3 V1 Cl1 83.30(5) . . ? Cl2 V1 Cl1 87.27(2) . . ? O1 V1 Cl1 92.91(7) . 2_666 ? O2 V1 Cl1 90.36(6) . 2_666 ? O3 V1 Cl1 82.41(5) . 2_666 ? Cl2 V1 Cl1 163.23(3) . 2_666 ? Cl1 V1 Cl1 78.49(2) . 2_666 ? V1 Cl1 V1 101.51(2) . 2_666 ? C1 O2 V1 124.00(16) . . ? C2 O3 C3 118.15(18) . . ? C2 O3 V1 107.65(14) . . ? C3 O3 V1 131.18(13) . . ? O2 C1 C2 110.5(2) . . ? O3 C2 C1 105.5(2) . . ? O3 C3 C5 111.3(2) . . ? O3 C3 C4 110.09(19) . . ? C5 C3 C4 113.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 V1 Cl1 V1 -91.27(7) . . . 2_666 ? O2 V1 Cl1 V1 58.30(17) . . . 2_666 ? O3 V1 Cl1 V1 83.58(5) . . . 2_666 ? Cl2 V1 Cl1 V1 171.10(3) . . . 2_666 ? Cl1 V1 Cl1 V1 0.0 2_666 . . 2_666 ? O1 V1 O2 C1 178.93(19) . . . . ? O3 V1 O2 C1 3.75(19) . . . . ? Cl2 V1 O2 C1 -81.14(19) . . . . ? Cl1 V1 O2 C1 29.4(3) . . . . ? Cl1 V1 O2 C1 85.92(19) 2_666 . . . ? O1 V1 O3 C2 -42.0(10) . . . . ? O2 V1 O3 C2 19.82(16) . . . . ? Cl2 V1 O3 C2 121.05(15) . . . . ? Cl1 V1 O3 C2 -151.37(15) . . . . ? Cl1 V1 O3 C2 -72.15(15) 2_666 . . . ? O1 V1 O3 C3 158.6(9) . . . . ? O2 V1 O3 C3 -139.6(2) . . . . ? Cl2 V1 O3 C3 -38.35(19) . . . . ? Cl1 V1 O3 C3 49.23(18) . . . . ? Cl1 V1 O3 C3 128.45(19) 2_666 . . . ? V1 O2 C1 C2 -26.0(3) . . . . ? C3 O3 C2 C1 127.0(2) . . . . ? V1 O3 C2 C1 -35.6(2) . . . . ? O2 C1 C2 O3 39.7(3) . . . . ? C2 O3 C3 C5 -59.4(3) . . . . ? V1 O3 C3 C5 98.2(2) . . . . ? C2 O3 C3 C4 67.1(3) . . . . ? V1 O3 C3 C4 -135.24(17) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.596 _refine_diff_density_min -0.832 _refine_diff_density_rms 0.108 #=== END data_5 _database_code_depnum_ccdc_archive 'CCDC 270040' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H22 Cl4 O6 V2' _chemical_formula_weight 481.96 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' V V 0.3005 0.5294 '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 7.0646(3) _cell_length_b 7.3724(2) _cell_length_c 10.2981(4) _cell_angle_alpha 70.6310(10) _cell_angle_beta 73.6510(10) _cell_angle_gamma 72.7450(10) _cell_volume 473.14(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.14 _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 244 _exptl_absorpt_coefficient_mu 1.572 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.184134 _exptl_absorpt_correction_T_max 0.811872 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3609 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.0946 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2148 _reflns_number_gt 1626 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0875P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2148 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1638 _refine_ls_wR_factor_gt 0.1535 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 V1 V 0.33756(11) 0.45358(10) 0.68288(7) 0.0193(2) Uani 1 1 d . . . Cl1 Cl 0.65138(16) 0.30283(16) 0.54626(11) 0.0271(3) Uani 1 1 d . . . Cl2 Cl 0.43360(19) 0.21891(17) 0.87213(12) 0.0323(3) Uani 1 1 d . . . O1 O 0.1928(5) 0.3512(5) 0.6530(4) 0.0290(7) Uani 1 1 d . . . O2 O 0.1529(4) 0.6251(4) 0.7638(3) 0.0224(7) Uani 1 1 d . . . O3 O 0.5206(5) 0.6335(5) 0.7162(4) 0.0270(7) Uani 1 1 d . . . C1 C 0.1873(7) 0.7725(7) 0.8143(5) 0.0294(10) Uani 1 1 d . . . C2 C 0.3896(7) 0.8206(7) 0.7304(6) 0.0314(11) Uani 1 1 d . . . H2A H 0.3754 0.9114 0.6389 0.080 Uiso 1 1 calc R . . H2B H 0.4429 0.8793 0.7800 0.080 Uiso 1 1 calc R . . C3 C 0.0142(9) 0.9528(8) 0.7870(7) 0.0454(14) Uani 1 1 d . . . H3A H 0.0157 1.0010 0.6880 0.080 Uiso 1 1 calc R . . H3B H 0.0301 1.0540 0.8198 0.080 Uiso 1 1 calc R . . H3C H -0.1124 0.9169 0.8361 0.080 Uiso 1 1 calc R . . C4 C 0.1887(9) 0.6808(9) 0.9696(6) 0.0404(13) Uani 1 1 d . . . H4A H 0.0631 0.6422 1.0172 0.080 Uiso 1 1 calc R . . H4B H 0.2053 0.7753 1.0086 0.080 Uiso 1 1 calc R . . H4C H 0.2987 0.5669 0.9812 0.080 Uiso 1 1 calc R . . C5 C 0.7308(7) 0.6377(9) 0.6793(6) 0.0384(13) Uani 1 1 d . . . H5A H 0.7573 0.7331 0.5905 0.080 Uiso 1 1 calc R . . H5B H 0.8112 0.5097 0.6725 0.080 Uiso 1 1 calc R . . H5C H 0.7648 0.6731 0.7502 0.080 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 V1 0.0144(4) 0.0188(4) 0.0252(4) -0.0059(3) -0.0050(3) -0.0035(3) Cl1 0.0214(6) 0.0235(5) 0.0285(5) -0.0054(4) -0.0063(4) 0.0057(4) Cl2 0.0361(7) 0.0256(6) 0.0296(6) -0.0008(4) -0.0099(5) -0.0031(5) O1 0.0229(17) 0.0296(17) 0.0390(18) -0.0117(14) -0.0056(14) -0.0102(14) O2 0.0166(15) 0.0234(15) 0.0284(15) -0.0094(12) -0.0041(12) -0.0042(12) O3 0.0147(15) 0.0321(18) 0.0384(18) -0.0138(14) -0.0047(13) -0.0072(13) C1 0.024(2) 0.025(2) 0.041(3) -0.017(2) -0.003(2) -0.0032(19) C2 0.025(2) 0.029(2) 0.047(3) -0.021(2) -0.001(2) -0.009(2) C3 0.034(3) 0.031(3) 0.070(4) -0.023(3) -0.002(3) -0.001(2) C4 0.038(3) 0.051(3) 0.037(3) -0.022(2) -0.001(2) -0.012(3) C5 0.013(2) 0.061(4) 0.050(3) -0.024(3) -0.006(2) -0.010(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 V1 O1 1.581(3) . ? V1 O2 1.762(3) . ? V1 Cl2 2.2501(12) . ? V1 O3 2.262(3) . ? V1 Cl1 2.4391(13) . ? V1 Cl1 2.4429(12) 2_666 ? Cl1 V1 2.4429(12) 2_666 ? O2 C1 1.453(6) . ? O3 C5 1.432(5) . ? O3 C2 1.443(6) . ? C1 C4 1.518(7) . ? C1 C2 1.522(7) . ? C1 C3 1.524(7) . ? 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 V1 O2 98.95(16) . . ? O1 V1 Cl2 98.84(13) . . ? O2 V1 Cl2 100.78(11) . . ? O1 V1 O3 173.40(15) . . ? O2 V1 O3 76.42(13) . . ? Cl2 V1 O3 86.74(9) . . ? O1 V1 Cl1 97.09(13) . . ? O2 V1 Cl1 161.25(11) . . ? Cl2 V1 Cl1 86.24(5) . . ? O3 V1 Cl1 86.75(9) . . ? O1 V1 Cl1 92.83(13) . 2_666 ? O2 V1 Cl1 90.97(11) . 2_666 ? Cl2 V1 Cl1 161.88(6) . 2_666 ? O3 V1 Cl1 82.64(9) . 2_666 ? Cl1 V1 Cl1 78.57(4) . 2_666 ? V1 Cl1 V1 101.43(4) . 2_666 ? C1 O2 V1 127.1(3) . . ? C5 O3 C2 112.8(4) . . ? C5 O3 V1 134.4(3) . . ? C2 O3 V1 108.5(3) . . ? O2 C1 C4 106.4(4) . . ? O2 C1 C2 107.7(4) . . ? C4 C1 C2 112.1(4) . . ? O2 C1 C3 106.6(4) . . ? C4 C1 C3 112.7(5) . . ? C2 C1 C3 110.9(4) . . ? O3 C2 C1 105.0(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.911 _refine_diff_density_min -1.265 _refine_diff_density_rms 0.162 #=== END data_6 _database_code_depnum_ccdc_archive 'CCDC 270041' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H18 Cl4 O6 V2' _chemical_formula_weight 477.92 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' V V 0.3005 0.5294 '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 19.8493(3) _cell_length_b 7.38780(10) _cell_length_c 13.38680(10) _cell_angle_alpha 90.00 _cell_angle_beta 118.1630(10) _cell_angle_gamma 90.00 _cell_volume 1730.66(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4737 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 30.56 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 1.718 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4137 _exptl_absorpt_correction_T_max 0.7251 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5897 _diffrn_reflns_av_R_equivalents 0.0839 _diffrn_reflns_av_sigmaI/netI 0.0803 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 26.49 _reflns_number_total 1792 _reflns_number_gt 1401 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0649P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1792 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1320 _refine_ls_wR_factor_gt 0.1247 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1882(2) 0.5925(5) 0.3098(3) 0.0360(10) Uani 1 1 d . . . H1A H 0.2298 0.6726 0.3151 0.043 Uiso 1 1 calc R . . H1B H 0.2060 0.5308 0.3836 0.043 Uiso 1 1 calc R . . C2 C 0.1178(3) 0.7050(6) 0.2840(3) 0.0357(10) Uani 1 1 d . . . H2 H 0.0823 0.6374 0.3042 0.043 Uiso 1 1 calc R . . C3 C 0.1360(3) 0.8904(5) 0.3391(4) 0.0369(10) Uani 1 1 d . . . H3A H 0.0970 0.9281 0.3611 0.044 Uiso 1 1 calc R . . H3B H 0.1868 0.8911 0.4072 0.044 Uiso 1 1 calc R . . C4 C 0.1351(3) 1.0123(6) 0.2487(4) 0.0501(14) Uani 1 1 d . . . H4A H 0.1857 1.0142 0.2509 0.060 Uiso 1 1 calc R . . H4B H 0.1210 1.1374 0.2577 0.060 Uiso 1 1 calc R . . C5 C 0.0756(2) 0.9299(5) 0.1398(3) 0.0324(9) Uani 1 1 d . . . H5A H 0.0238 0.9736 0.1214 0.039 Uiso 1 1 calc R . . H5B H 0.0858 0.9592 0.0761 0.039 Uiso 1 1 calc R . . O1 O 0.12001(18) 0.3204(4) 0.0278(3) 0.0382(7) Uani 1 1 d . . . O2 O 0.17109(15) 0.4612(3) 0.2230(2) 0.0287(6) Uani 1 1 d . . . O3 O 0.08264(15) 0.7370(3) 0.1628(2) 0.0269(6) Uani 1 1 d . . . Cl1 Cl -0.00118(5) 0.37957(12) 0.09446(7) 0.0267(3) Uani 1 1 d . . . Cl2 Cl 0.18065(6) 0.69177(14) 0.04094(9) 0.0366(3) Uani 1 1 d . . . V1 V 0.10711(3) 0.50208(8) 0.07845(5) 0.0224(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 0.035(2) 0.037(2) 0.018(2) 0.0016(16) -0.0020(17) 0.0017(18) C2 0.045(2) 0.034(2) 0.018(2) 0.0009(16) 0.0070(19) -0.0041(18) C3 0.052(3) 0.028(2) 0.025(2) -0.0064(16) 0.013(2) -0.0056(19) C4 0.062(3) 0.028(2) 0.032(3) 0.0023(18) -0.002(2) -0.007(2) C5 0.042(2) 0.0192(18) 0.025(2) 0.0033(15) 0.0073(18) 0.0070(17) O1 0.0471(18) 0.0312(15) 0.0329(17) -0.0031(12) 0.0162(15) 0.0072(13) O2 0.0262(14) 0.0267(13) 0.0226(14) 0.0045(11) 0.0028(11) 0.0033(11) O3 0.0369(15) 0.0195(12) 0.0142(13) 0.0013(9) 0.0037(12) 0.0031(11) Cl1 0.0280(5) 0.0269(5) 0.0158(4) 0.0047(3) 0.0027(4) -0.0043(4) Cl2 0.0290(5) 0.0437(6) 0.0357(6) 0.0041(4) 0.0143(5) -0.0049(4) V1 0.0229(4) 0.0211(4) 0.0168(4) 0.0007(2) 0.0042(3) 0.0014(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 C1 O2 1.427(5) . ? C1 C2 1.520(6) . ? C2 O3 1.451(5) . ? C2 C3 1.517(5) . ? C3 C4 1.503(6) . ? C4 C5 1.505(6) . ? C5 O3 1.451(4) . ? O1 V1 1.578(3) . ? O2 V1 1.768(3) . ? O3 V1 2.245(3) . ? Cl1 V1 2.4331(11) . ? Cl1 V1 2.4392(10) 5_565 ? Cl2 V1 2.2447(12) . ? V1 Cl1 2.4392(10) 5_565 ? 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 C2 110.3(3) . . ? O3 C2 C3 106.0(3) . . ? O3 C2 C1 104.4(3) . . ? C3 C2 C1 113.6(4) . . ? C4 C3 C2 103.9(3) . . ? C3 C4 C5 104.1(4) . . ? O3 C5 C4 103.8(3) . . ? C1 O2 V1 123.2(2) . . ? C2 O3 C5 110.1(3) . . ? C2 O3 V1 109.4(2) . . ? C5 O3 V1 132.5(2) . . ? V1 Cl1 V1 100.65(4) . 5_565 ? O1 V1 O2 98.40(14) . . ? O1 V1 Cl2 100.39(12) . . ? O2 V1 Cl2 98.30(9) . . ? O1 V1 O3 172.29(14) . . ? O2 V1 O3 78.24(11) . . ? Cl2 V1 O3 87.01(8) . . ? O1 V1 Cl1 92.90(12) . . ? O2 V1 Cl1 92.77(9) . . ? Cl2 V1 Cl1 161.21(5) . . ? O3 V1 Cl1 80.41(7) . . ? O1 V1 Cl1 98.01(11) . 5_565 ? O2 V1 Cl1 162.12(10) . 5_565 ? Cl2 V1 Cl1 85.66(4) . 5_565 ? O3 V1 Cl1 84.60(7) . 5_565 ? Cl1 V1 Cl1 79.35(4) . 5_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.927 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.143 #=== END data_7 _database_code_depnum_ccdc_archive 'CCDC 270042' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H15 Cl2 O4 V' _chemical_formula_weight 285.03 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' V V 0.3005 0.5294 '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 11.1610(2) _cell_length_b 7.6550(1) _cell_length_c 13.7459(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.533(2) _cell_angle_gamma 90.00 _cell_volume 1150.83(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7057 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 30.55 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 1.312 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.618368 _exptl_absorpt_correction_T_max 0.839966 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8556 _diffrn_reflns_av_R_equivalents 0.0913 _diffrn_reflns_av_sigmaI/netI 0.0914 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2636 _reflns_number_gt 2157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0433P)^2^+0.0838P] 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 2636 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1253 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.20814(4) 0.20563(6) 0.81837(4) 0.02236(17) Uani 1 1 d . . . Cl2 Cl 0.39179(7) 0.14712(10) 0.92086(6) 0.0305(2) Uani 1 1 d . . . Cl1 Cl 0.22322(8) -0.04068(10) 0.72745(6) 0.0364(2) Uani 1 1 d . . . O2 O 0.0986(2) 0.3114(3) 0.72342(17) 0.0311(5) Uani 1 1 d . . . O4 O 0.22504(18) 0.4483(3) 0.88801(17) 0.0275(5) Uani 1 1 d . . . O3 O 0.33015(19) 0.3413(3) 0.72342(16) 0.0268(5) Uani 1 1 d . . . O1 O 0.1186(2) 0.1356(3) 0.88494(18) 0.0345(5) Uani 1 1 d . . . C4 C 0.1207(3) 0.5211(4) 0.9245(3) 0.0324(7) Uani 1 1 d . . . H4A H 0.1026 0.4503 0.9801 0.039 Uiso 1 1 calc R . . H4B H 0.0470 0.5247 0.8709 0.039 Uiso 1 1 calc R . . C5 C 0.1597(3) 0.7020(4) 0.9588(3) 0.0351(8) Uani 1 1 d . . . H5A H 0.1250 0.7359 1.0169 0.042 Uiso 1 1 calc R . . H5B H 0.1340 0.7883 0.9050 0.042 Uiso 1 1 calc R . . C6 C 0.2984(3) 0.6886(4) 0.9862(3) 0.0347(8) Uani 1 1 d . . . H6A H 0.3372 0.8044 0.9840 0.042 Uiso 1 1 calc R . . H6B H 0.3253 0.6377 1.0532 0.042 Uiso 1 1 calc R . . C7 C 0.3277(3) 0.5693(4) 0.9074(3) 0.0300(7) Uani 1 1 d . . . H7A H 0.3340 0.6356 0.8467 0.036 Uiso 1 1 calc R . . H7B H 0.4055 0.5065 0.9314 0.036 Uiso 1 1 calc R . . C3 C 0.4473(3) 0.2836(5) 0.7080(3) 0.0374(8) Uani 1 1 d . . . H3A H 0.4379 0.1724 0.6720 0.056 Uiso 1 1 calc R . . H3B H 0.5026 0.2678 0.7723 0.056 Uiso 1 1 calc R . . H3C H 0.4813 0.3713 0.6692 0.056 Uiso 1 1 calc R . . C2 C 0.2510(3) 0.3852(5) 0.6305(3) 0.0385(8) Uani 1 1 d . . . H2A H 0.2399 0.2836 0.5851 0.046 Uiso 1 1 calc R . . H2B H 0.2854 0.4834 0.5980 0.046 Uiso 1 1 calc R . . C1 C 0.1332(3) 0.4360(5) 0.6569(3) 0.0395(8) Uani 1 1 d . . . H1A H 0.1413 0.5528 0.6884 0.047 Uiso 1 1 calc R . . H1B H 0.0689 0.4428 0.5959 0.047 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 V1 0.0169(3) 0.0218(3) 0.0291(3) 0.0003(2) 0.0064(2) -0.00214(18) Cl2 0.0262(4) 0.0343(4) 0.0296(4) 0.0051(3) 0.0024(3) 0.0059(3) Cl1 0.0423(5) 0.0275(4) 0.0393(5) -0.0065(3) 0.0080(4) 0.0002(3) O2 0.0199(11) 0.0329(12) 0.0390(13) -0.0004(10) 0.0022(10) -0.0010(8) O4 0.0145(10) 0.0280(11) 0.0426(13) -0.0090(9) 0.0117(9) -0.0028(8) O3 0.0203(11) 0.0308(11) 0.0304(12) 0.0029(9) 0.0078(9) 0.0039(8) O1 0.0288(12) 0.0338(12) 0.0445(14) -0.0017(10) 0.0162(11) -0.0112(9) C4 0.0205(15) 0.0324(17) 0.048(2) -0.0065(15) 0.0154(14) 0.0025(12) C5 0.0359(19) 0.0253(16) 0.050(2) -0.0020(15) 0.0224(16) 0.0029(13) C6 0.0333(18) 0.0329(17) 0.0385(19) -0.0085(14) 0.0091(15) -0.0080(13) C7 0.0189(15) 0.0270(15) 0.0447(19) -0.0049(14) 0.0075(13) -0.0078(11) C3 0.0229(16) 0.048(2) 0.045(2) 0.0101(16) 0.0168(15) 0.0053(14) C2 0.037(2) 0.048(2) 0.0308(18) 0.0147(16) 0.0068(15) 0.0063(15) C1 0.0311(18) 0.046(2) 0.040(2) 0.0129(17) 0.0046(15) 0.0060(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 V1 O1 1.578(2) . ? V1 O2 1.794(2) . ? V1 O4 2.081(2) . ? V1 Cl1 2.2868(9) . ? V1 Cl2 2.2879(9) . ? V1 O3 2.312(2) . ? O2 C1 1.427(4) . ? O4 C7 1.456(3) . ? O4 C4 1.467(3) . ? O3 C3 1.435(4) . ? O3 C2 1.440(4) . ? C4 C5 1.499(4) . ? C5 C6 1.521(5) . ? C6 C7 1.503(5) . ? C2 C1 1.484(5) . ? 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 V1 O2 99.02(12) . . ? O1 V1 O4 92.67(10) . . ? O2 V1 O4 85.28(10) . . ? O1 V1 Cl1 99.26(9) . . ? O2 V1 Cl1 95.07(8) . . ? O4 V1 Cl1 167.85(7) . . ? O1 V1 Cl2 99.78(9) . . ? O2 V1 Cl2 158.95(8) . . ? O4 V1 Cl2 84.47(6) . . ? Cl1 V1 Cl2 91.18(3) . . ? O1 V1 O3 173.10(10) . . ? O2 V1 O3 77.23(9) . . ? O4 V1 O3 81.32(8) . . ? Cl1 V1 O3 86.91(6) . . ? Cl2 V1 O3 83.07(6) . . ? C1 O2 V1 122.4(2) . . ? C7 O4 C4 110.2(2) . . ? C7 O4 V1 130.38(18) . . ? C4 O4 V1 119.42(17) . . ? C3 O3 C2 110.9(3) . . ? C3 O3 V1 126.98(19) . . ? C2 O3 V1 106.23(19) . . ? O4 C4 C5 104.9(2) . . ? C4 C5 C6 103.5(3) . . ? C7 C6 C5 102.6(3) . . ? O4 C7 C6 104.0(3) . . ? O3 C2 C1 105.2(3) . . ? O2 C1 C2 110.4(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.728 _refine_diff_density_min -1.090 _refine_diff_density_rms 0.129 #=== END data_8 _database_code_depnum_ccdc_archive 'CCDC 270043' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H17 Cl1 O4 V' _chemical_formula_weight 299.06 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pna2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 15.0823(7) _cell_length_b 7.4876(3) _cell_length_c 11.1036(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1253.93(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1799 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 30.52 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 1.209 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7441 _exptl_absorpt_correction_T_max 0.9095 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7375 _diffrn_reflns_av_R_equivalents 0.1321 _diffrn_reflns_av_sigmaI/netI 0.0982 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2167 _reflns_number_gt 1657 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(6) _refine_ls_number_reflns 2167 _refine_ls_number_parameters 137 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1269 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 C1 C 0.2567(5) 0.3449(12) 0.8232(8) 0.045(2) Uani 1 1 d . . . H1A H 0.2966 0.2405 0.8310 0.053 Uiso 1 1 calc R . . H1B H 0.2608 0.4156 0.8984 0.053 Uiso 1 1 calc R . . C2 C 0.2853(5) 0.4563(11) 0.7197(6) 0.0361(19) Uani 1 1 d . . . H2A H 0.2636 0.5802 0.7292 0.043 Uiso 1 1 calc R . . H2B H 0.3508 0.4588 0.7143 0.043 Uiso 1 1 calc R . . C3 C 0.2905(4) 0.4291(11) 0.5024(7) 0.0324(18) Uani 1 1 d . . . H3A H 0.3075 0.5566 0.5062 0.039 Uiso 1 1 calc R . . H3B H 0.2478 0.4142 0.4355 0.039 Uiso 1 1 calc R . . C4 C 0.3715(5) 0.3179(14) 0.4780(8) 0.057(3) Uani 1 1 d . . . H4A H 0.4122 0.3263 0.5466 0.085 Uiso 1 1 calc R . . H4B H 0.4011 0.3619 0.4053 0.085 Uiso 1 1 calc R . . H4C H 0.3540 0.1931 0.4662 0.085 Uiso 1 1 calc R . . C5 C 0.0798(5) 0.5900(9) 0.5450(6) 0.0282(16) Uani 1 1 d . . . H5A H 0.0912 0.5349 0.4655 0.034 Uiso 1 1 calc R . . H5B H 0.1306 0.6672 0.5666 0.034 Uiso 1 1 calc R . . C6 C -0.0055(5) 0.6958(10) 0.5434(7) 0.0365(19) Uani 1 1 d . . . H6A H 0.0046 0.8196 0.5152 0.044 Uiso 1 1 calc R . . H6B H -0.0506 0.6383 0.4914 0.044 Uiso 1 1 calc R . . C7 C -0.0331(5) 0.6924(8) 0.6730(8) 0.0366(16) Uani 1 1 d . . . H7A H -0.0980 0.7091 0.6808 0.044 Uiso 1 1 calc R . . H7B H -0.0026 0.7873 0.7191 0.044 Uiso 1 1 calc R . . C8 C -0.0059(5) 0.5104(11) 0.7170(7) 0.0391(18) Uani 1 1 d . . . H8A H 0.0154 0.5167 0.8012 0.047 Uiso 1 1 calc R . . H8B H -0.0564 0.4262 0.7130 0.047 Uiso 1 1 calc R . . O1 O 0.0384(3) 0.1220(6) 0.7096(4) 0.0302(12) Uani 1 1 d . . . O2 O 0.1679(3) 0.2852(6) 0.8066(4) 0.0266(11) Uani 1 1 d . . . O3 O 0.2487(3) 0.3778(7) 0.6147(4) 0.0264(11) Uani 1 1 d . . . O4 O 0.0653(3) 0.4533(6) 0.6367(4) 0.0260(11) Uani 1 1 d . . . Cl1 Cl 0.22066(10) -0.0354(2) 0.6695(2) 0.0346(4) Uani 1 1 d . . . Cl2 Cl 0.11216(11) 0.1707(2) 0.45954(15) 0.0300(4) Uani 1 1 d . . . V1 V 0.12813(6) 0.20739(13) 0.66418(10) 0.0214(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 0.041(5) 0.053(6) 0.040(5) 0.003(4) -0.020(4) -0.013(4) C2 0.036(5) 0.045(5) 0.027(4) -0.001(4) -0.008(4) -0.012(4) C3 0.018(4) 0.049(5) 0.030(4) 0.014(4) 0.005(3) -0.005(3) C4 0.034(5) 0.092(7) 0.044(5) 0.009(5) 0.005(4) 0.006(5) C5 0.026(4) 0.028(4) 0.032(4) 0.010(3) -0.001(3) 0.003(3) C6 0.043(5) 0.034(4) 0.033(5) -0.003(3) -0.007(4) 0.010(4) C7 0.037(4) 0.032(4) 0.042(4) -0.011(4) -0.001(5) 0.003(3) C8 0.036(4) 0.037(4) 0.044(4) -0.001(3) 0.023(4) 0.005(3) O1 0.020(2) 0.032(3) 0.038(3) 0.000(2) 0.003(2) -0.007(2) O2 0.032(3) 0.027(3) 0.021(2) 0.001(2) 0.005(2) -0.003(2) O3 0.016(2) 0.038(3) 0.025(2) -0.003(2) -0.001(2) -0.006(2) O4 0.024(2) 0.028(2) 0.026(3) 0.0011(19) 0.007(2) 0.0022(19) Cl1 0.0367(9) 0.0265(8) 0.0405(9) -0.0019(11) -0.0032(11) 0.0081(7) Cl2 0.0273(8) 0.0362(9) 0.0266(9) -0.0065(8) -0.0045(8) 0.0051(8) V1 0.0181(5) 0.0209(5) 0.0251(6) -0.0015(6) -0.0003(6) -0.0018(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 C1 O2 1.425(9) . ? C1 C2 1.484(11) . ? C2 O3 1.418(8) . ? C3 O3 1.449(8) . ? C3 C4 1.502(10) . ? C5 O4 1.460(8) . ? C5 C6 1.511(9) . ? C6 C7 1.498(11) . ? C7 C8 1.504(10) . ? C8 O4 1.459(8) . ? O1 V1 1.579(4) . ? O2 V1 1.788(4) . ? O3 V1 2.288(4) . ? O4 V1 2.093(4) . ? Cl1 V1 2.2927(17) . ? Cl2 V1 2.3096(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 C2 110.4(6) . . ? O3 C2 C1 106.9(6) . . ? O3 C3 C4 111.3(6) . . ? O4 C5 C6 104.4(5) . . ? C7 C6 C5 102.5(6) . . ? C6 C7 C8 104.6(6) . . ? O4 C8 C7 105.5(6) . . ? C1 O2 V1 122.1(5) . . ? C2 O3 C3 115.3(5) . . ? C2 O3 V1 110.1(4) . . ? C3 O3 V1 134.5(4) . . ? C8 O4 C5 109.3(5) . . ? C8 O4 V1 120.1(4) . . ? C5 O4 V1 130.6(4) . . ? O1 V1 O2 97.9(2) . . ? O1 V1 O4 90.8(2) . . ? O2 V1 O4 89.65(19) . . ? O1 V1 O3 169.5(2) . . ? O2 V1 O3 76.38(18) . . ? O4 V1 O3 80.47(17) . . ? O1 V1 Cl1 101.09(18) . . ? O2 V1 Cl1 91.81(16) . . ? O4 V1 Cl1 167.66(13) . . ? O3 V1 Cl1 87.97(13) . . ? O1 V1 Cl2 100.19(18) . . ? O2 V1 Cl2 161.24(16) . . ? O4 V1 Cl2 85.06(13) . . ? O3 V1 Cl2 84.98(12) . . ? Cl1 V1 Cl2 89.68(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.406 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.093 #=== END data_9 _database_code_depnum_ccdc_archive 'CCDC 270044' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H19 Cl1 O4 V' _chemical_formula_weight 313.08 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pna2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 19.711(5) _cell_length_b 9.880(5) _cell_length_c 7.039(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 1370.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4686 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 30.59 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.92 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 1.109 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.484970 _exptl_absorpt_correction_T_max 0.920577 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9980 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3034 _reflns_number_gt 2628 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SIR97 - J. Appl. Cryst. (1999) 32, 115-119' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0449P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(3) _refine_ls_number_reflns 3034 _refine_ls_number_parameters 147 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.006 _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 V1 V 0.40735(2) 0.15944(5) 0.42228(7) 0.02928(12) Uani 1 1 d . . . Cl2 Cl 0.36091(3) 0.36552(7) 0.33946(11) 0.03551(17) Uani 1 1 d . . . Cl1 Cl 0.34690(5) 0.05606(9) 0.18628(10) 0.0484(2) Uani 1 1 d . . . O3 O 0.31369(9) 0.13929(18) 0.6225(3) 0.0256(4) Uani 1 1 d . . . O4 O 0.44324(9) 0.2618(2) 0.6612(3) 0.0345(5) Uani 1 1 d . . . O2 O 0.42357(11) 0.0070(2) 0.5492(3) 0.0363(5) Uani 1 1 d . . . O1 O 0.47785(11) 0.1721(2) 0.3167(3) 0.0461(6) Uani 1 1 d . . . C2 C 0.31029(14) -0.0003(3) 0.6761(5) 0.0338(6) Uani 1 1 d . . . H2A H 0.2883 -0.0549 0.5755 0.041 Uiso 1 1 calc R . . H2B H 0.2845 -0.0116 0.7959 0.041 Uiso 1 1 calc R . . C7 C 0.46468(15) 0.4268(4) 0.8930(4) 0.0425(8) Uani 1 1 d . . . H7A H 0.4511 0.4558 1.0221 0.051 Uiso 1 1 calc R . . H7B H 0.4784 0.5072 0.8185 0.051 Uiso 1 1 calc R . . C3 C 0.24904(14) 0.2126(3) 0.6278(4) 0.0326(6) Uani 1 1 d . . . H3 H 0.2587 0.3085 0.5910 0.039 Uiso 1 1 calc R . . C1 C 0.38305(16) -0.0415(3) 0.7020(4) 0.0394(7) Uani 1 1 d . . . H1A H 0.4004 -0.0045 0.8233 0.047 Uiso 1 1 calc R . . H1B H 0.3861 -0.1415 0.7080 0.047 Uiso 1 1 calc R . . C6 C 0.40833(15) 0.3502(4) 0.7956(5) 0.0383(7) Uani 1 1 d . . . H6A H 0.3818 0.2967 0.8884 0.046 Uiso 1 1 calc R . . H6B H 0.3774 0.4130 0.7285 0.046 Uiso 1 1 calc R . . C4 C 0.22053(15) 0.2152(3) 0.8264(5) 0.0402(7) Uani 1 1 d . . . H4A H 0.2031 0.1252 0.8590 0.060 Uiso 1 1 calc R . . H4B H 0.1836 0.2814 0.8332 0.060 Uiso 1 1 calc R . . H4C H 0.2564 0.2404 0.9161 0.060 Uiso 1 1 calc R . . C8 C 0.52119(15) 0.3226(4) 0.9007(6) 0.0490(9) Uani 1 1 d . . . H8A H 0.5661 0.3672 0.9066 0.059 Uiso 1 1 calc R . . H8B H 0.5160 0.2631 1.0129 0.059 Uiso 1 1 calc R . . C9 C 0.51379(16) 0.2433(4) 0.7203(5) 0.0487(9) Uani 1 1 d . . . H9A H 0.5452 0.2778 0.6218 0.058 Uiso 1 1 calc R . . H9B H 0.5236 0.1463 0.7426 0.058 Uiso 1 1 calc R . . C5 C 0.19961(19) 0.1568(4) 0.4844(5) 0.0534(10) Uani 1 1 d . . . H5A H 0.2209 0.1553 0.3586 0.080 Uiso 1 1 calc R . . H5B H 0.1591 0.2142 0.4806 0.080 Uiso 1 1 calc R . . H5C H 0.1867 0.0646 0.5208 0.080 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 V1 0.0336(2) 0.0303(2) 0.0239(2) 0.0027(2) 0.0079(2) 0.00942(18) Cl2 0.0368(4) 0.0306(3) 0.0392(4) 0.0115(3) 0.0039(3) 0.0044(3) Cl1 0.0765(6) 0.0448(5) 0.0239(3) -0.0052(4) 0.0002(4) 0.0005(4) O3 0.0266(9) 0.0212(10) 0.0289(9) 0.0008(7) 0.0032(7) 0.0037(7) O4 0.0228(10) 0.0432(12) 0.0373(11) -0.0055(10) 0.0012(8) 0.0064(8) O2 0.0436(12) 0.0358(12) 0.0295(9) 0.0034(9) 0.0103(9) 0.0183(9) O1 0.0454(13) 0.0539(14) 0.0391(12) 0.0100(11) 0.0199(10) 0.0160(10) C2 0.0463(17) 0.0217(13) 0.0335(14) 0.0011(12) 0.0031(14) 0.0040(11) C7 0.0389(17) 0.056(2) 0.0331(17) -0.0044(14) 0.0019(12) -0.0133(14) C3 0.0234(13) 0.0288(15) 0.0456(17) 0.0042(13) 0.0057(11) 0.0061(11) C1 0.0487(17) 0.0381(17) 0.0314(14) 0.0116(14) 0.0134(14) 0.0145(14) C6 0.0293(15) 0.053(2) 0.0330(15) -0.0123(13) 0.0010(11) 0.0017(13) C4 0.0359(16) 0.0342(17) 0.0506(18) -0.0062(15) 0.0125(14) 0.0062(13) C8 0.0312(15) 0.066(2) 0.050(2) 0.0094(18) -0.0109(15) -0.0067(15) C9 0.0273(16) 0.059(2) 0.060(2) 0.0065(18) -0.0069(14) 0.0097(14) C5 0.0374(18) 0.077(3) 0.0457(19) 0.0104(18) -0.0072(14) 0.0025(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O1 1.581(2) . ? V1 O2 1.780(2) . ? V1 O4 2.086(2) . ? V1 Cl1 2.2853(13) . ? V1 Cl2 2.3072(12) . ? V1 O3 2.331(2) . ? O3 C2 1.432(3) . ? O3 C3 1.466(3) . ? O4 C6 1.460(4) . ? O4 C9 1.463(4) . ? O2 C1 1.423(4) . ? C2 C1 1.502(4) . ? C7 C6 1.509(4) . ? C7 C8 1.517(5) . ? C3 C4 1.507(5) . ? C3 C5 1.508(5) . ? C8 C9 1.499(5) . ? 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 V1 O2 98.32(11) . . ? O1 V1 O4 92.43(11) . . ? O2 V1 O4 86.83(10) . . ? O1 V1 Cl1 98.74(11) . . ? O2 V1 Cl1 94.60(9) . . ? O4 V1 Cl1 168.40(6) . . ? O1 V1 Cl2 99.23(9) . . ? O2 V1 Cl2 160.87(7) . . ? O4 V1 Cl2 84.87(7) . . ? Cl1 V1 Cl2 90.23(4) . . ? O1 V1 O3 170.79(11) . . ? O2 V1 O3 76.50(8) . . ? O4 V1 O3 79.78(8) . . ? Cl1 V1 O3 89.34(7) . . ? Cl2 V1 O3 85.07(5) . . ? C2 O3 C3 115.4(2) . . ? C2 O3 V1 106.18(15) . . ? C3 O3 V1 131.40(16) . . ? C6 O4 C9 109.8(2) . . ? C6 O4 V1 130.73(16) . . ? C9 O4 V1 119.43(19) . . ? C1 O2 V1 124.30(17) . . ? O3 C2 C1 104.4(2) . . ? C6 C7 C8 102.5(3) . . ? O3 C3 C4 110.9(2) . . ? O3 C3 C5 111.3(3) . . ? C4 C3 C5 112.7(3) . . ? O2 C1 C2 110.7(2) . . ? O4 C6 C7 104.3(2) . . ? C9 C8 C7 104.6(3) . . ? O4 C9 C8 105.6(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.246 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.056 #=== END data_10 _database_code_depnum_ccdc_archive 'CCDC 270045' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H19 Cl2 O4 V' _chemical_formula_weight 313.08 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' V V 0.3005 0.5294 '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 7.7037(4) _cell_length_b 17.0284(9) _cell_length_c 10.6692(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.583(2) _cell_angle_gamma 90.00 _cell_volume 1341.39(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2622 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 30.56 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 1.134 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5902 _exptl_absorpt_correction_T_max 0.9455 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9092 _diffrn_reflns_av_R_equivalents 0.1031 _diffrn_reflns_av_sigmaI/netI 0.0806 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2626 _reflns_number_gt 1779 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0639P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2626 _refine_ls_number_parameters 148 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0859 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1083 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _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 0.0411(5) 0.2289(2) 0.9072(4) 0.0190(8) Uani 1 1 d . . . C2 C 0.2278(5) 0.2143(2) 1.0016(4) 0.0198(8) Uani 1 1 d . . . H2A H 0.3092 0.2592 1.0013 0.024 Uiso 1 1 calc R . . H2B H 0.2194 0.2067 1.0917 0.024 Uiso 1 1 calc R . . C3 C 0.4685(5) 0.1226(3) 1.0406(4) 0.0294(10) Uani 1 1 d . . . H3A H 0.5545 0.1656 1.0446 0.044 Uiso 1 1 calc R . . H3B H 0.5118 0.0753 1.0068 0.044 Uiso 1 1 calc R . . H3C H 0.4579 0.1122 1.1285 0.044 Uiso 1 1 calc R . . C4 C -0.1014(5) 0.1724(3) 0.9268(4) 0.0286(10) Uani 1 1 d . . . H4A H -0.2146 0.1800 0.8570 0.043 Uiso 1 1 calc R . . H4B H -0.1225 0.1825 1.0117 0.043 Uiso 1 1 calc R . . H4C H -0.0593 0.1183 0.9243 0.043 Uiso 1 1 calc R . . C5 C -0.0148(6) 0.3144(3) 0.9168(4) 0.0311(10) Uani 1 1 d . . . H5A H 0.0728 0.3493 0.8941 0.047 Uiso 1 1 calc R . . H5B H -0.0178 0.3255 1.0063 0.047 Uiso 1 1 calc R . . H5C H -0.1353 0.3232 0.8561 0.047 Uiso 1 1 calc R . . C6 C -0.1259(5) 0.0626(3) 0.6259(4) 0.0250(9) Uani 1 1 d . . . H6A H -0.1196 0.0745 0.5365 0.030 Uiso 1 1 calc R . . H6B H -0.2049 0.1019 0.6507 0.030 Uiso 1 1 calc R . . C7 C -0.1968(6) -0.0191(2) 0.6327(4) 0.0310(10) Uani 1 1 d . . . H7A H -0.1621 -0.0547 0.5705 0.037 Uiso 1 1 calc R . . H7B H -0.3302 -0.0193 0.6143 0.037 Uiso 1 1 calc R . . C8 C -0.1043(6) -0.0424(3) 0.7735(4) 0.0323(10) Uani 1 1 d . . . H8A H -0.1661 -0.0190 0.8342 0.039 Uiso 1 1 calc R . . H8B H -0.1004 -0.1002 0.7843 0.039 Uiso 1 1 calc R . . C9 C 0.0834(6) -0.0087(2) 0.7951(4) 0.0295(10) Uani 1 1 d . . . H9A H 0.1403 0.0026 0.8890 0.035 Uiso 1 1 calc R . . H9B H 0.1617 -0.0455 0.7642 0.035 Uiso 1 1 calc R . . O1 O 0.1484(4) 0.17422(16) 0.5751(3) 0.0247(6) Uani 1 1 d . . . O2 O 0.0566(3) 0.21767(15) 0.7761(2) 0.0184(6) Uani 1 1 d . . . O3 O 0.2941(3) 0.14435(16) 0.9554(2) 0.0197(6) Uani 1 1 d . . . O4 O 0.0550(3) 0.06317(16) 0.7189(3) 0.0229(6) Uani 1 1 d . . . Cl2 Cl 0.44143(13) 0.06787(6) 0.73824(10) 0.0289(3) Uani 1 1 d . . . Cl1 Cl 0.43569(13) 0.25878(6) 0.77267(10) 0.0281(3) Uani 1 1 d . . . V1 V 0.22187(8) 0.16196(4) 0.72803(6) 0.01715(19) 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 0.0207(19) 0.019(2) 0.0176(19) -0.0047(15) 0.0057(16) 0.0032(16) C2 0.0231(19) 0.015(2) 0.021(2) -0.0038(15) 0.0064(17) 0.0004(16) C3 0.024(2) 0.030(3) 0.030(2) 0.0053(18) -0.0003(18) 0.0080(19) C4 0.022(2) 0.037(3) 0.030(2) -0.0029(19) 0.0131(18) -0.0005(18) C5 0.035(2) 0.026(3) 0.032(2) -0.0060(18) 0.008(2) 0.0085(19) C6 0.019(2) 0.028(2) 0.025(2) -0.0021(17) 0.0010(17) -0.0024(17) C7 0.027(2) 0.024(3) 0.043(3) -0.0136(19) 0.011(2) -0.0059(19) C8 0.033(2) 0.020(2) 0.045(3) -0.0022(19) 0.014(2) -0.0048(19) C9 0.031(2) 0.015(2) 0.041(2) 0.0076(18) 0.008(2) 0.0010(18) O1 0.0289(15) 0.0230(17) 0.0231(14) 0.0002(12) 0.0091(12) -0.0010(12) O2 0.0199(13) 0.0144(15) 0.0205(14) -0.0002(10) 0.0053(11) 0.0023(11) O3 0.0183(13) 0.0174(15) 0.0220(14) 0.0008(11) 0.0038(11) 0.0036(11) O4 0.0198(13) 0.0147(15) 0.0308(15) 0.0022(11) 0.0018(12) -0.0001(11) Cl2 0.0247(5) 0.0272(6) 0.0372(6) -0.0004(4) 0.0130(5) 0.0090(4) Cl1 0.0284(5) 0.0259(6) 0.0306(6) 0.0016(4) 0.0095(4) -0.0089(4) V1 0.0189(3) 0.0142(4) 0.0194(3) 0.0005(3) 0.0071(3) 0.0016(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 C1 O2 1.449(4) . ? C1 C4 1.518(5) . ? C1 C2 1.522(5) . ? C1 C5 1.531(5) . ? C2 O3 1.437(4) . ? C3 O3 1.439(5) . ? C6 O4 1.462(5) . ? C6 C7 1.505(6) . ? C7 C8 1.520(6) . ? C8 C9 1.511(6) . ? C9 O4 1.451(5) . ? O1 V1 1.581(3) . ? O2 V1 1.777(2) . ? O3 V1 2.348(3) . ? O4 V1 2.103(3) . ? Cl2 V1 2.3096(12) . ? Cl1 V1 2.2827(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 C4 108.1(3) . . ? O2 C1 C2 107.1(3) . . ? C4 C1 C2 113.0(3) . . ? O2 C1 C5 107.0(3) . . ? C4 C1 C5 111.4(3) . . ? C2 C1 C5 110.0(3) . . ? O3 C2 C1 105.6(3) . . ? O4 C6 C7 105.2(3) . . ? C6 C7 C8 102.4(3) . . ? C9 C8 C7 102.1(3) . . ? O4 C9 C8 104.5(3) . . ? C1 O2 V1 127.7(2) . . ? C2 O3 C3 110.8(3) . . ? C2 O3 V1 104.2(2) . . ? C3 O3 V1 126.1(2) . . ? C9 O4 C6 109.7(3) . . ? C9 O4 V1 131.0(2) . . ? C6 O4 V1 119.2(2) . . ? O1 V1 O2 98.77(13) . . ? O1 V1 O4 91.37(13) . . ? O2 V1 O4 87.78(11) . . ? O1 V1 Cl1 98.31(11) . . ? O2 V1 Cl1 95.05(9) . . ? O4 V1 Cl1 169.37(8) . . ? O1 V1 Cl2 100.49(11) . . ? O2 V1 Cl2 158.78(9) . . ? O4 V1 Cl2 82.94(8) . . ? Cl1 V1 Cl2 90.92(4) . . ? O1 V1 O3 173.03(12) . . ? O2 V1 O3 75.39(10) . . ? O4 V1 O3 84.67(10) . . ? Cl1 V1 O3 86.13(7) . . ? Cl2 V1 O3 84.74(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.674 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.110 #=== END data_Si _database_code_depnum_ccdc_archive 'CCDC 270046' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H33 O1 Si3 V1' _chemical_formula_weight 328.59 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6(3)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 10.51890(10) _cell_length_b 10.51890(10) _cell_length_c 10.0831(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 966.20(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7011 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 30.54 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 348 _exptl_absorpt_coefficient_mu 0.684 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.593339 _exptl_absorpt_correction_T_max 0.826275 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6519 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.94 _reflns_number_total 668 _reflns_number_gt 653 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0000P)^2^+5.0905P] 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 668 _refine_ls_number_parameters 46 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0724 _refine_ls_wR_factor_ref 0.1753 _refine_ls_wR_factor_gt 0.1751 _refine_ls_goodness_of_fit_ref 1.377 _refine_ls_restrained_S_all 1.374 _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 C1 C 0.9243(7) 0.7960(7) 0.2500 0.0226(14) Uani 1 2 d SD . . C2 C 1.1547(7) 0.7537(7) 0.0990(6) 0.0443(15) Uani 1 1 d . . . H2A H 1.0931 0.7215 0.0193 0.066 Uiso 1 1 calc R . . H2B H 1.2144 0.7062 0.1024 0.066 Uiso 1 1 calc R . . H2C H 1.2192 0.8605 0.0963 0.066 Uiso 1 1 calc R . . C3 C 0.9093(10) 0.4980(9) 0.2500 0.044(2) Uani 1 2 d SD . . O1 O 1.0000 1.0000 0.0000 0.022(3) Uani 0.485(6) 6 d SP . 1 V1 V 1.0000 1.0000 0.1756(2) 0.0166(8) Uani 0.485(6) 3 d SP . 1 Si1 Si 1.0349(2) 0.7022(2) 0.2500 0.0225(6) Uani 1 2 d S . . H1 H 0.854(7) 0.770(9) 0.178(6) 0.11(3) Uiso 1 1 d D . . H3B H 0.853(7) 0.473(8) 0.170(4) 0.07(2) Uiso 1 1 d D . . H3A H 0.966(9) 0.449(9) 0.2500 0.06(3) Uiso 1 2 d SD . . 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 0.024(3) 0.018(3) 0.028(3) 0.000 0.000 0.013(3) C2 0.049(3) 0.051(4) 0.045(3) 0.011(3) 0.015(3) 0.034(3) C3 0.040(5) 0.019(4) 0.072(6) 0.000 0.000 0.014(4) O1 0.024(5) 0.024(5) 0.020(8) 0.000 0.000 0.012(2) V1 0.0158(9) 0.0158(9) 0.0180(14) 0.000 0.000 0.0079(4) Si1 0.0225(10) 0.0198(10) 0.0272(10) 0.000 0.000 0.0121(8) _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 Si1 1.864(7) . ? C1 V1 2.023(6) 10_556 ? C1 V1 2.023(6) . ? C2 Si1 1.875(6) . ? C3 Si1 1.877(8) . ? O1 V1 1.771(2) 7_775 ? O1 V1 1.771(2) . ? V1 V1 1.499(5) 10_556 ? V1 C1 2.023(6) 2_765 ? V1 C1 2.023(6) 3_675 ? Si1 C2 1.875(6) 10_556 ? 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 Si1 C1 V1 122.9(3) . 10_556 ? Si1 C1 V1 122.9(3) . . ? V1 C1 V1 43.50(18) 10_556 . ? V1 O1 V1 180.0 7_775 . ? V1 V1 O1 180.000(1) 10_556 . ? V1 V1 C1 68.25(9) 10_556 2_765 ? O1 V1 C1 111.75(9) . 2_765 ? V1 V1 C1 68.25(9) 10_556 3_675 ? O1 V1 C1 111.75(9) . 3_675 ? C1 V1 C1 107.10(10) 2_765 3_675 ? V1 V1 C1 68.25(9) 10_556 . ? O1 V1 C1 111.75(9) . . ? C1 V1 C1 107.10(10) 2_765 . ? C1 V1 C1 107.10(10) 3_675 . ? C1 Si1 C2 110.7(2) . 10_556 ? C1 Si1 C2 110.7(2) . . ? C2 Si1 C2 108.6(4) 10_556 . ? C1 Si1 C3 109.7(4) . . ? C2 Si1 C3 108.5(2) 10_556 . ? C2 Si1 C3 108.5(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.787 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.101