Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email GALINDO@US.ES _publ_contact_author_name 'Prof Agustin Galindo' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name A.Galindo 'D.del Rio' A.Ienco D.Masi C.Mealli R.Vicente data_die1 _database_code_CSD 202077 _audit_creation_date 2002-10-18T12:31:14-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C4 H8 O8 V1' _chemical_formula_sum 'C4 H8 O8 V' _chemical_formula_weight 235.04 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'A b a 2' _symmetry_space_group_name_Hall 'A 2 -2ac' _symmetry_Int_Tables_number 41 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/2, y+1, z+1/2' 'x+1/2, -y+1, z+1/2' _cell_length_a 8.919(3) _cell_length_b 10.889(2) _cell_length_c 8.593(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 834.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 16 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.204 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_unetI/netI 0.0141 _diffrn_reflns_number 399 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 24.95 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 399 _reflns_number_gt 388 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0662P)^2^+0.1269P] 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_number_reflns 399 _refine_ls_number_parameters 63 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0245 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0652 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(4) _refine_diff_density_max 0.225 _refine_diff_density_min -0.49 _refine_diff_density_rms 0.089 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 1 0 0.79302(12) 0.0223(3) Uani 1 2 d S . . O2 O 1 0 1.0463(6) 0.0335(13) Uani 1 2 d S . . O3 O 1.1235(3) 0.14542(19) 0.8615(3) 0.0294(5) Uani 1 1 d . . . O4 O 0.8106(2) 0.1050(2) 0.8048(3) 0.0317(5) Uani 1 1 d . . . O5 O 1 0 0.6084(6) 0.0382(13) Uani 1 2 d S . . O6 O 1.2162(3) 0.26657(17) 1.0452(4) 0.0327(5) Uani 1 1 d . . . C1 C 1.1420(3) 0.1757(3) 1.0027(4) 0.0245(6) Uani 1 1 d . . . C2 C 1.0701(3) 0.0978(3) 1.1266(4) 0.0254(6) Uani 1 1 d . . . H2A H 1.1451 0.0667 1.1983 0.050(10) Uiso 1 1 calc R . . H2B H 0.9969 0.145 1.1848 0.050(10) Uiso 1 1 calc R . . H41 H 0.7961 0.1464 0.8798 0.05 Uiso 1 1 d . . . H42 H 0.7762 0.1429 0.7199 0.05 Uiso 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 V1 0.0323(4) 0.0195(4) 0.0152(4) 0 0 0.0004(2) O2 0.058(3) 0.028(2) 0.015(3) 0 0 -0.0200(12) O3 0.0436(13) 0.0233(11) 0.0212(10) -0.0034(9) 0.0050(10) -0.0072(9) O4 0.0404(11) 0.0308(12) 0.0239(10) 0.0024(10) 0.0028(10) 0.0088(9) O5 0.053(3) 0.046(3) 0.016(3) 0 0 0.0140(14) O6 0.0459(11) 0.0247(11) 0.0273(10) -0.0049(12) 0.0059(16) -0.0126(9) C1 0.0283(12) 0.0214(14) 0.0239(14) -0.0009(12) 0.0024(12) 0.0002(11) C2 0.0328(14) 0.0214(15) 0.0219(15) -0.0044(13) -0.0002(13) -0.0062(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O5 1.586(5) . ? V1 O3 2.017(2) . ? V1 O3 2.017(2) 2_755 ? V1 O4 2.042(2) 2_755 ? V1 O4 2.042(2) . ? V1 O2 2.176(5) . ? O2 C2 1.414(4) . ? O2 C2 1.414(4) 2_755 ? O3 C1 1.268(4) . ? O4 H41 0.797 . ? O4 H42 0.8926 . ? O6 C1 1.246(4) . ? C1 C2 1.505(4) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? 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 O5 V1 O3 106.95(9) . . ? O5 V1 O3 106.95(9) . 2_755 ? O3 V1 O3 146.09(17) . 2_755 ? O5 V1 O4 92.84(9) . 2_755 ? O3 V1 O4 88.46(9) . 2_755 ? O3 V1 O4 89.88(9) 2_755 2_755 ? O5 V1 O4 92.84(9) . . ? O3 V1 O4 89.88(9) . . ? O3 V1 O4 88.46(9) 2_755 . ? O4 V1 O4 174.32(17) 2_755 . ? O5 V1 O2 180.0000(10) . . ? O3 V1 O2 73.05(8) . . ? O3 V1 O2 73.05(8) 2_755 . ? O4 V1 O2 87.16(9) 2_755 . ? O4 V1 O2 87.16(9) . . ? C2 O2 C2 121.6(4) . 2_755 ? C2 O2 V1 119.2(2) . . ? C2 O2 V1 119.2(2) 2_755 . ? C1 O3 V1 123.6(2) . . ? V1 O4 H41 119.4 . . ? V1 O4 H42 120.2 . . ? H41 O4 H42 110.1 . . ? O6 C1 O3 123.8(3) . . ? O6 C1 C2 117.8(3) . . ? O3 C1 C2 118.4(2) . . ? O2 C2 C1 105.5(3) . . ? O2 C2 H2A 110.6 . . ? C1 C2 H2A 110.6 . . ? O2 C2 H2B 110.6 . . ? C1 C2 H2B 110.6 . . ? H2A C2 H2B 108.8 . . ? #======================================END data_die44 _database_code_CSD 202078 _audit_creation_date 2002-10-22T16:47:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H24 N4 O12 V2, 2(H2 O)' _chemical_formula_sum 'C28 H28 N4 O14 V2' _chemical_formula_weight 746.42 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.995(5) _cell_length_b 10.784(5) _cell_length_c 19.143(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.010(5) _cell_angle_gamma 90.00 _cell_volume 3016.3(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_factor_mur 4.895 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Linear fit to sin(theta)/lambda - 12 parameters ; _exptl_absorpt_correction_T_min 0.274 _exptl_absorpt_correction_T_max 0.9523 _exptl_absorpt_correction_t_ave 0.5275 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_unetI/netI 0.0685 _diffrn_reflns_number 4321 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 22.98 _diffrn_reflns_theta_full 22.98 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 4180 _reflns_number_gt 2749 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0682P)^2^+12.5431P] 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_number_reflns 4180 _refine_ls_number_parameters 446 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1261 _refine_ls_R_factor_gt 0.0711 _refine_ls_wR_factor_ref 0.1934 _refine_ls_wR_factor_gt 0.1722 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.097 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 1.177 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.115 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.64603(8) 0.24474(13) 0.97612(7) 0.0323(4) Uani 1 1 d . . . O1 O 0.6476(3) 0.3624(6) 0.8977(3) 0.0405(14) Uani 1 1 d . . . O2 O 0.6156(4) 0.5443(6) 0.8392(4) 0.0620(18) Uani 1 1 d . . . O3 O 0.6057(3) 0.4337(5) 1.0111(3) 0.0334(13) Uani 1 1 d . . . O4 O 0.7597(3) 0.3114(5) 1.0562(3) 0.0387(13) Uani 1 1 d . . . O5 O 0.8257(4) 0.4167(6) 1.1649(3) 0.0523(16) Uani 1 1 d . . . O6 O 0.6827(4) 0.1223(6) 0.9529(3) 0.0532(16) Uani 1 1 d . . . C1 C 0.6227(5) 0.4747(9) 0.8919(5) 0.041(2) Uani 1 1 d . . . C2 C 0.5986(5) 0.5250(8) 0.9552(4) 0.043(2) Uani 1 1 d . . . H2A H 0.6391 0.5936 0.9799 0.052 Uiso 1 1 calc R . . H2B H 0.5365 0.5568 0.9331 0.052 Uiso 1 1 calc R . . C3 C 0.6716(5) 0.4615(8) 1.0871(4) 0.042(2) Uani 1 1 d . . . H3A H 0.6466 0.4384 1.1237 0.05 Uiso 1 1 calc R . . H3B H 0.6832 0.55 1.0916 0.05 Uiso 1 1 calc R . . C4 C 0.7613(5) 0.3926(8) 1.1057(5) 0.039(2) Uani 1 1 d . . . N1 N 0.5024(4) 0.2281(6) 0.9163(3) 0.0286(14) Uani 1 1 d . . . N2 N 0.6064(4) 0.1749(6) 1.0600(3) 0.0321(15) Uani 1 1 d . . . C5 C 0.4549(5) 0.2538(8) 0.8423(5) 0.041(2) Uani 1 1 d . . . H5 H 0.4859 0.2812 0.8134 0.05 Uiso 1 1 calc R . . C6 C 0.3603(5) 0.2406(8) 0.8075(5) 0.045(2) Uani 1 1 d . . . H6 H 0.3286 0.2574 0.7557 0.055 Uiso 1 1 calc R . . C7 C 0.3151(5) 0.2032(8) 0.8498(5) 0.042(2) Uani 1 1 d . . . H7 H 0.2517 0.1962 0.8277 0.051 Uiso 1 1 calc R . . C8 C 0.3638(5) 0.1752(8) 0.9262(5) 0.042(2) Uani 1 1 d . . . H8 H 0.3333 0.1476 0.9556 0.051 Uiso 1 1 calc R . . C9 C 0.4579(5) 0.1885(7) 0.9590(4) 0.0308(18) Uani 1 1 d . . . C10 C 0.5148(5) 0.1592(7) 1.0390(4) 0.0291(17) Uani 1 1 d . . . C11 C 0.4821(5) 0.1174(8) 1.0904(5) 0.042(2) Uani 1 1 d . . . H11 H 0.4194 0.1078 1.0755 0.051 Uiso 1 1 calc R . . C12 C 0.5411(6) 0.0897(8) 1.1636(5) 0.049(2) Uani 1 1 d . . . H12 H 0.5188 0.0631 1.199 0.059 Uiso 1 1 calc R . . C13 C 0.6351(6) 0.1016(9) 1.1847(5) 0.054(2) Uani 1 1 d . . . H13 H 0.6768 0.0817 1.2338 0.064 Uiso 1 1 calc R . . C14 C 0.6638(5) 0.1433(8) 1.1312(4) 0.041(2) Uani 1 1 d . . . H14 H 0.7264 0.1502 1.1445 0.049 Uiso 1 1 calc R . . V2 V 0.33388(8) 0.24089(13) 0.48915(8) 0.0370(4) Uani 1 1 d . . . O7 O 0.2978(3) 0.3116(5) 0.5680(3) 0.0408(14) Uani 1 1 d . . . O8 O 0.3324(4) 0.4290(6) 0.6713(3) 0.0504(16) Uani 1 1 d . . . O9 O 0.4091(3) 0.4316(5) 0.5204(3) 0.0350(13) Uani 1 1 d . . . O10 O 0.2550(3) 0.3578(6) 0.4093(3) 0.0443(15) Uani 1 1 d . . . O11 O 0.2296(4) 0.5355(6) 0.3471(3) 0.0653(19) Uani 1 1 d . . . O12 O 0.2766(4) 0.1177(5) 0.4683(4) 0.0552(17) Uani 1 1 d . . . C15 C 0.3422(5) 0.4005(8) 0.6135(5) 0.038(2) Uani 1 1 d . . . C16 C 0.4120(5) 0.4684(8) 0.5933(4) 0.041(2) Uani 1 1 d . . . H16A H 0.4008 0.5569 0.5927 0.05 Uiso 1 1 calc R . . H16B H 0.4727 0.4523 0.6324 0.05 Uiso 1 1 calc R . . C17 C 0.3638(5) 0.5165(8) 0.4594(4) 0.045(2) Uani 1 1 d . . . H17A H 0.4043 0.5362 0.4346 0.054 Uiso 1 1 calc R . . H17B H 0.3519 0.5928 0.4806 0.054 Uiso 1 1 calc R . . C18 C 0.2749(5) 0.4677(9) 0.4004(5) 0.041(2) Uani 1 1 d . . . N3 N 0.4568(4) 0.1749(6) 0.5734(4) 0.0400(17) Uani 1 1 d . . . N4 N 0.4163(4) 0.2194(6) 0.4278(4) 0.0366(16) Uani 1 1 d . . . C19 C 0.4706(6) 0.1494(8) 0.6465(5) 0.049(2) Uani 1 1 d . . . H19 H 0.4222 0.1595 0.6611 0.059 Uiso 1 1 calc R . . C20 C 0.5546(6) 0.1085(9) 0.7010(5) 0.053(2) Uani 1 1 d . . . H20 H 0.5634 0.0927 0.7512 0.064 Uiso 1 1 calc R . . C21 C 0.6235(6) 0.0928(9) 0.6767(6) 0.059(3) Uani 1 1 d . . . H21 H 0.6804 0.0656 0.7115 0.071 Uiso 1 1 calc R . . C22 C 0.6109(5) 0.1160(8) 0.6030(5) 0.048(2) Uani 1 1 d . . . H22 H 0.6587 0.1047 0.5878 0.057 Uiso 1 1 calc R . . C23 C 0.5264(5) 0.1564(7) 0.5512(4) 0.0346(19) Uani 1 1 d . . . C24 C 0.5055(5) 0.1813(7) 0.4714(5) 0.0359(19) Uani 1 1 d . . . C25 C 0.5656(5) 0.1686(8) 0.4367(5) 0.042(2) Uani 1 1 d . . . H25 H 0.6254 0.143 0.4655 0.051 Uiso 1 1 calc R . . C26 C 0.5387(6) 0.1929(8) 0.3612(5) 0.048(2) Uani 1 1 d . . . H26 H 0.5802 0.1862 0.3386 0.058 Uiso 1 1 calc R . . C27 C 0.4499(5) 0.2275(8) 0.3182(5) 0.046(2) Uani 1 1 d . . . H27 H 0.4298 0.2427 0.266 0.055 Uiso 1 1 calc R . . C28 C 0.3910(6) 0.2390(8) 0.3547(5) 0.047(2) Uani 1 1 d . . . H28 H 0.3306 0.2618 0.3257 0.056 Uiso 1 1 calc R . . O13 O 0.6247(5) 0.4263(12) 0.7095(5) 0.116(3) Uani 1 1 d D . . H13A H 0.639(6) 0.466(9) 0.755(3) 0.09 Uiso 1 1 d D . . H13B H 0.678(4) 0.409(10) 0.705(5) 0.09 Uiso 1 1 d D . . O14 O 0.4180(6) 0.6162(9) 0.7801(5) 0.091(3) Uani 1 1 d D . . H14A H 0.386(5) 0.565(8) 0.741(4) 0.09 Uiso 1 1 d D . . H14B H 0.476(2) 0.601(10) 0.787(5) 0.09 Uiso 1 1 d 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 V1 0.0191(6) 0.0411(8) 0.0407(8) -0.0059(7) 0.0163(6) -0.0014(6) O1 0.033(3) 0.052(4) 0.048(3) -0.001(3) 0.029(3) -0.003(3) O2 0.067(4) 0.071(5) 0.055(4) 0.017(4) 0.031(4) -0.005(4) O3 0.022(3) 0.042(3) 0.037(3) -0.002(3) 0.013(2) 0.002(2) O4 0.018(3) 0.049(3) 0.050(3) -0.007(3) 0.014(2) 0.000(2) O5 0.036(3) 0.067(4) 0.041(3) -0.005(3) 0.001(3) -0.007(3) O6 0.037(3) 0.054(4) 0.073(4) -0.014(3) 0.026(3) 0.002(3) C1 0.020(4) 0.054(6) 0.049(6) 0.005(5) 0.013(4) -0.011(4) C2 0.029(4) 0.050(6) 0.043(5) 0.005(4) 0.006(4) 0.002(4) C3 0.041(5) 0.048(6) 0.037(5) -0.006(4) 0.017(4) 0.000(4) C4 0.028(4) 0.048(6) 0.047(5) 0.006(5) 0.020(4) -0.002(4) N1 0.025(3) 0.037(4) 0.027(3) 0.000(3) 0.014(3) -0.002(3) N2 0.022(3) 0.039(4) 0.033(4) 0.002(3) 0.009(3) 0.002(3) C5 0.034(4) 0.049(5) 0.044(5) -0.009(4) 0.020(4) -0.009(4) C6 0.036(5) 0.058(6) 0.035(5) -0.006(4) 0.007(4) -0.008(4) C7 0.021(4) 0.054(6) 0.045(5) -0.006(4) 0.005(4) 0.000(4) C8 0.029(4) 0.053(6) 0.050(5) -0.002(4) 0.020(4) -0.006(4) C9 0.026(4) 0.029(4) 0.039(5) -0.006(4) 0.014(4) 0.002(3) C10 0.028(4) 0.032(4) 0.034(4) -0.004(3) 0.020(4) -0.004(3) C11 0.035(5) 0.053(6) 0.048(5) -0.002(4) 0.025(4) -0.002(4) C12 0.057(6) 0.054(6) 0.046(6) 0.007(5) 0.031(5) 0.001(5) C13 0.052(6) 0.060(6) 0.037(5) 0.016(5) 0.006(4) 0.011(5) C14 0.027(4) 0.050(5) 0.036(5) 0.007(4) 0.004(4) 0.007(4) V2 0.0180(6) 0.0440(9) 0.0494(9) -0.0045(7) 0.0140(6) -0.0022(7) O7 0.030(3) 0.043(3) 0.052(4) -0.005(3) 0.020(3) -0.005(3) O8 0.045(3) 0.073(4) 0.039(3) 0.000(3) 0.023(3) 0.002(3) O9 0.022(3) 0.045(3) 0.037(3) 0.001(3) 0.011(2) -0.001(2) O10 0.022(3) 0.055(4) 0.052(4) -0.003(3) 0.010(3) 0.004(3) O11 0.059(4) 0.070(5) 0.045(4) 0.007(4) -0.001(3) 0.016(4) O12 0.042(3) 0.044(4) 0.081(5) -0.014(3) 0.027(3) -0.012(3) C15 0.018(4) 0.047(5) 0.048(5) 0.008(4) 0.010(4) 0.012(4) C16 0.030(4) 0.057(6) 0.036(5) -0.002(4) 0.012(4) 0.000(4) C17 0.037(5) 0.054(6) 0.040(5) 0.001(4) 0.012(4) -0.011(4) C18 0.035(5) 0.049(6) 0.044(5) -0.009(5) 0.022(4) 0.004(5) N3 0.035(4) 0.040(4) 0.051(5) 0.006(3) 0.024(3) 0.002(3) N4 0.027(3) 0.041(4) 0.043(4) 0.000(3) 0.015(3) 0.004(3) C19 0.048(5) 0.048(6) 0.058(6) 0.007(5) 0.028(5) 0.008(4) C20 0.046(5) 0.060(6) 0.059(6) 0.013(5) 0.026(5) 0.008(5) C21 0.034(5) 0.066(7) 0.065(7) 0.013(5) 0.006(5) -0.004(5) C22 0.030(5) 0.057(6) 0.056(6) 0.012(5) 0.016(4) 0.004(4) C23 0.027(4) 0.029(4) 0.051(5) -0.001(4) 0.020(4) -0.003(4) C24 0.023(4) 0.034(5) 0.048(5) -0.013(4) 0.012(4) -0.003(4) C25 0.027(4) 0.050(6) 0.052(6) -0.004(4) 0.019(4) -0.003(4) C26 0.038(5) 0.061(6) 0.054(6) -0.010(5) 0.026(4) -0.004(4) C27 0.037(5) 0.059(6) 0.038(5) -0.008(4) 0.011(4) 0.003(4) C28 0.034(4) 0.057(6) 0.046(5) -0.007(5) 0.011(4) -0.002(4) O13 0.060(5) 0.202(11) 0.070(6) -0.012(6) 0.009(4) 0.016(6) O14 0.079(5) 0.107(7) 0.090(6) -0.029(5) 0.036(5) -0.002(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O6 1.580(6) . ? V1 O1 1.973(6) . ? V1 O4 1.976(5) . ? V1 N2 2.092(6) . ? V1 N1 2.117(6) . ? V1 O3 2.316(5) . ? O1 C1 1.266(10) . ? O2 C1 1.224(10) . ? O3 C2 1.424(9) . ? O3 C3 1.439(9) . ? O4 C4 1.283(10) . ? O5 C4 1.209(9) . ? C1 C2 1.514(12) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.524(11) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? N1 C5 1.335(9) . ? N1 C9 1.353(9) . ? N2 C14 1.340(9) . ? N2 C10 1.363(9) . ? C5 C6 1.390(11) . ? C5 H5 0.93 . ? C6 C7 1.348(11) . ? C6 H6 0.93 . ? C7 C8 1.383(11) . ? C7 H7 0.93 . ? C8 C9 1.382(10) . ? C8 H8 0.93 . ? C9 C10 1.464(10) . ? C10 C11 1.365(10) . ? C11 C12 1.367(11) . ? C11 H11 0.93 . ? C12 C13 1.395(12) . ? C12 H12 0.93 . ? C13 C14 1.359(11) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? V2 O12 1.571(6) . ? V2 O7 1.975(5) . ? V2 O10 1.987(6) . ? V2 N3 2.096(7) . ? V2 N4 2.104(6) . ? V2 O9 2.334(5) . ? O7 C15 1.296(10) . ? O8 C15 1.219(9) . ? O9 C17 1.427(9) . ? O9 C16 1.434(9) . ? O10 C18 1.257(10) . ? O11 C18 1.225(10) . ? C15 C16 1.510(11) . ? C16 H16A 0.97 . ? C16 H16B 0.97 . ? C17 C18 1.507(11) . ? C17 H17A 0.97 . ? C17 H17B 0.97 . ? N3 C19 1.354(10) . ? N3 C23 1.358(9) . ? N4 C28 1.307(10) . ? N4 C24 1.391(9) . ? C19 C20 1.394(12) . ? C19 H19 0.93 . ? C20 C21 1.369(12) . ? C20 H20 0.93 . ? C21 C22 1.365(12) . ? C21 H21 0.93 . ? C22 C23 1.382(11) . ? C22 H22 0.93 . ? C23 C24 1.449(11) . ? C24 C25 1.381(10) . ? C25 C26 1.356(11) . ? C25 H25 0.93 . ? C26 C27 1.371(11) . ? C26 H26 0.93 . ? C27 C28 1.389(11) . ? C27 H27 0.93 . ? C28 H28 0.93 . ? O13 H13A 0.90(2) . ? O13 H13B 0.90(2) . ? O14 H14A 0.91(2) . ? O14 H14B 0.90(2) . ? 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 O6 V1 O1 101.6(3) . . ? O6 V1 O4 101.1(3) . . ? O1 V1 O4 93.7(2) . . ? O6 V1 N2 100.3(3) . . ? O1 V1 N2 156.5(2) . . ? O4 V1 N2 90.3(2) . . ? O6 V1 N1 102.8(3) . . ? O1 V1 N1 89.4(2) . . ? O4 V1 N1 154.7(2) . . ? N2 V1 N1 77.5(2) . . ? O6 V1 O3 174.3(2) . . ? O1 V1 O3 75.3(2) . . ? O4 V1 O3 74.5(2) . . ? N2 V1 O3 83.6(2) . . ? N1 V1 O3 82.1(2) . . ? C1 O1 V1 125.5(5) . . ? C2 O3 C3 114.7(6) . . ? C2 O3 V1 109.8(4) . . ? C3 O3 V1 107.5(4) . . ? C4 O4 V1 123.9(5) . . ? O2 C1 O1 125.4(8) . . ? O2 C1 C2 118.1(9) . . ? O1 C1 C2 116.5(7) . . ? O3 C2 C1 112.6(7) . . ? O3 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? O3 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? O3 C3 C4 111.6(6) . . ? O3 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? O3 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 108 . . ? O5 C4 O4 126.3(7) . . ? O5 C4 C3 118.5(8) . . ? O4 C4 C3 115.2(7) . . ? C5 N1 C9 119.6(6) . . ? C5 N1 V1 125.4(5) . . ? C9 N1 V1 115.0(5) . . ? C14 N2 C10 118.5(6) . . ? C14 N2 V1 125.1(5) . . ? C10 N2 V1 116.3(5) . . ? N1 C5 C6 121.7(7) . . ? N1 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C7 C6 C5 119.2(8) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C8 119.5(7) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 C9 119.8(7) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? N1 C9 C8 120.2(7) . . ? N1 C9 C10 116.4(6) . . ? C8 C9 C10 123.5(7) . . ? N2 C10 C11 120.7(7) . . ? N2 C10 C9 114.7(6) . . ? C11 C10 C9 124.6(7) . . ? C10 C11 C12 120.2(7) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 119.3(8) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 117.9(8) . . ? C14 C13 H13 121.1 . . ? C12 C13 H13 121.1 . . ? N2 C14 C13 123.3(7) . . ? N2 C14 H14 118.4 . . ? C13 C14 H14 118.4 . . ? O12 V2 O7 101.5(3) . . ? O12 V2 O10 102.7(3) . . ? O7 V2 O10 93.0(2) . . ? O12 V2 N3 100.1(3) . . ? O7 V2 N3 91.0(2) . . ? O10 V2 N3 155.6(3) . . ? O12 V2 N4 101.4(3) . . ? O7 V2 N4 155.9(2) . . ? O10 V2 N4 89.2(2) . . ? N3 V2 N4 77.7(2) . . ? O12 V2 O9 175.6(2) . . ? O7 V2 O9 75.2(2) . . ? O10 V2 O9 74.8(2) . . ? N3 V2 O9 83.0(2) . . ? N4 V2 O9 82.3(2) . . ? C15 O7 V2 123.2(5) . . ? C17 O9 C16 115.0(6) . . ? C17 O9 V2 108.6(4) . . ? C16 O9 V2 107.6(4) . . ? C18 O10 V2 125.9(5) . . ? O8 C15 O7 124.0(7) . . ? O8 C15 C16 119.5(8) . . ? O7 C15 C16 116.6(7) . . ? O9 C16 C15 112.3(7) . . ? O9 C16 H16A 109.1 . . ? C15 C16 H16A 109.1 . . ? O9 C16 H16B 109.1 . . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? O9 C17 C18 113.5(7) . . ? O9 C17 H17A 108.9 . . ? C18 C17 H17A 108.9 . . ? O9 C17 H17B 108.9 . . ? C18 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? O11 C18 O10 125.4(8) . . ? O11 C18 C17 118.3(9) . . ? O10 C18 C17 116.2(8) . . ? C19 N3 C23 118.9(7) . . ? C19 N3 V2 124.9(5) . . ? C23 N3 V2 116.2(5) . . ? C28 N4 C24 119.1(7) . . ? C28 N4 V2 126.1(5) . . ? C24 N4 V2 114.8(5) . . ? N3 C19 C20 122.7(8) . . ? N3 C19 H19 118.7 . . ? C20 C19 H19 118.7 . . ? C21 C20 C19 116.7(9) . . ? C21 C20 H20 121.7 . . ? C19 C20 H20 121.7 . . ? C22 C21 C20 121.9(9) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 119.3(8) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? N3 C23 C22 120.6(7) . . ? N3 C23 C24 115.8(7) . . ? C22 C23 C24 123.6(7) . . ? C25 C24 N4 119.0(8) . . ? C25 C24 C23 125.6(7) . . ? N4 C24 C23 115.3(6) . . ? C26 C25 C24 120.9(8) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C27 119.6(8) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C26 C27 C28 118.1(8) . . ? C26 C27 H27 121 . . ? C28 C27 H27 121 . . ? N4 C28 C27 123.2(8) . . ? N4 C28 H28 118.4 . . ? C27 C28 H28 118.4 . . ? H13A O13 H13B 108(5) . . ? H14A O14 H14B 103(4) . . ? #================================================================END data_die88 _database_code_CSD 202079 _audit_creation_date 2002-10-22T15:26:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C10 H14 O14 V2, 2(H2O), 2Na' _chemical_formula_sum 'C10 H18 Na2 O16 V2' _chemical_formula_weight 546.14 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c 21' _symmetry_space_group_name_Hall 'C 2c -2' _symmetry_Int_Tables_number 36 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, 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' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 15.884(5) _cell_length_b 6.860(5) _cell_length_c 18.394(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2004.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9 _cell_measurement_theta_max 15 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.053 _exptl_absorpt_factor_mur 0.105 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 1 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.7861 _exptl_absorpt_correction_T_max 0.8987 _exptl_absorpt_correction_t_ave 0.8661 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_UB_11 0.02409 _diffrn_orient_matrix_UB_12 0.050505 _diffrn_orient_matrix_UB_13 -0.031326 _diffrn_orient_matrix_UB_21 -0.084167 _diffrn_orient_matrix_UB_22 -0.024797 _diffrn_orient_matrix_UB_23 -0.038874 _diffrn_orient_matrix_UB_31 -0.116625 _diffrn_orient_matrix_UB_32 0.028291 _diffrn_orient_matrix_UB_33 0.021528 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 1 _diffrn_standards_decay_corr_max 1.017 _diffrn_standards_decay_corr_min 0.994 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 3 -5 -1 -3 5 1 3 -5 _diffrn_reflns_av_unetI/netI 0.0486 _diffrn_reflns_number 1053 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.97 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 1053 _reflns_number_gt 898 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1000P)^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_number_reflns 1053 _refine_ls_number_parameters 123 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.067 _refine_ls_wR_factor_ref 0.1707 _refine_ls_wR_factor_gt 0.1597 _refine_ls_goodness_of_fit_ref 1.288 _refine_ls_restrained_S_all 1.287 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(8) _refine_diff_density_max 1.374 _refine_diff_density_min -0.832 _refine_diff_density_rms 0.165 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' 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 0.5 0.7891(3) 0.78159(12) 0.0219(5) Uani 1 2 d S . . V2 V 0.5 0.6549(3) 0.62067(12) 0.0215(5) Uani 1 2 d S . . Na1 Na 0.2344(3) 1.3521(5) 0.9172(2) 0.0338(10) Uani 1 1 d . . . O1 O 0.5 0.5985(13) 0.8317(6) 0.030(2) Uani 1 2 d S . . O2 O 0.4047(5) 0.9194(10) 0.8349(4) 0.0338(17) Uani 1 1 d . . . O3 O 0.5 1.0993(13) 0.7425(5) 0.025(2) Uani 1 2 d S . . O4 O 0.5 0.9856(14) 0.5894(5) 0.026(2) Uani 1 2 d S . . O5 O 0.5919(5) 0.6915(10) 0.5467(4) 0.0300(17) Uani 1 1 d . . . O6 O 0.5 0.4240(12) 0.6213(7) 0.034(2) Uani 1 2 d S . . O7 O 0.6881(5) 0.8803(11) 0.4941(6) 0.047(2) Uani 1 1 d . . . O8 O 0.1401(4) 1.0756(11) 0.9376(5) 0.041(2) Uani 1 1 d . . . O10 O 0.3038(5) 1.1461(12) 0.8337(5) 0.045(2) Uani 1 1 d . . . O9 O 0.5759(4) 0.7310(11) 0.7004(4) 0.0291(15) Uani 1 1 d . . . C1 C 0.3734(6) 1.0831(14) 0.8135(6) 0.030(2) Uiso 1 1 d . . . C2 C 0.4240(7) 1.1977(16) 0.7603(6) 0.035(2) Uiso 1 1 d . . . H2A H 0.3912 1.2183 0.7165 0.07(2) Uiso 1 1 calc R . . H2B H 0.4371 1.3243 0.7809 0.07(2) Uiso 1 1 calc R . . C3 C 0.6232(7) 0.8569(15) 0.5286(6) 0.031(2) Uiso 1 1 d . . . C4 C 0.5741(9) 1.030(2) 0.5525(8) 0.057(4) Uiso 1 1 d . . . H4A H 0.6093 1.1096 0.5838 0.07(2) Uiso 1 1 calc R . . H4B H 0.5602 1.108 0.5101 0.07(2) Uiso 1 1 calc R . . C5 C 0.6668(10) 0.693(2) 0.7045(9) 0.059(4) Uiso 1 1 d . . . H5A H 0.6775 0.5582 0.6948 0.32(13) Uiso 1 1 calc R . . H5B H 0.6868 0.7254 0.7523 0.32(13) Uiso 1 1 calc R . . H5C H 0.6955 0.7721 0.6692 0.32(13) 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 0.0287(12) 0.0086(9) 0.0283(12) 0.0004(9) 0 0 V2 0.0274(11) 0.0084(9) 0.0285(12) 0.0002(10) 0 0 Na1 0.032(2) 0.0172(18) 0.052(3) -0.0026(18) 0.0063(19) 0.0009(16) O1 0.048(6) 0.013(4) 0.029(5) 0.006(4) 0 0 O2 0.046(4) 0.017(3) 0.038(4) 0.002(3) 0.012(3) 0.008(3) O3 0.030(5) 0.012(4) 0.034(6) -0.002(4) 0 0 O4 0.028(5) 0.013(4) 0.038(5) 0.000(4) 0 0 O5 0.041(4) 0.008(3) 0.041(4) -0.003(3) 0.010(3) 0.000(3) O6 0.045(5) 0.009(4) 0.049(6) 0.000(5) 0 0 O7 0.045(5) 0.024(4) 0.074(6) 0.004(4) 0.022(5) -0.009(3) O8 0.029(3) 0.027(4) 0.068(6) 0.010(4) -0.010(4) -0.007(3) O10 0.035(4) 0.040(5) 0.060(5) -0.006(4) 0.007(4) 0.006(3) O9 0.029(3) 0.027(4) 0.032(3) -0.001(3) -0.005(3) 0.001(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 1.600(9) . ? V1 O9 1.961(8) 3_655 ? V1 O9 1.961(8) . ? V1 O2 2.012(7) 3_655 ? V1 O2 2.012(7) . ? V1 O3 2.247(9) . ? V1 V2 3.100(3) . ? V2 O6 1.584(9) . ? V2 O9 1.968(7) . ? V2 O9 1.968(7) 3_655 ? V2 O5 2.011(7) 3_655 ? V2 O5 2.011(7) . ? V2 O4 2.340(10) . ? Na1 O10 2.362(9) . ? Na1 O7 2.431(9) 8_475 ? Na1 O8 2.446(8) . ? Na1 O7 2.461(10) 2_675 ? Na1 O8 2.542(9) 7 ? Na1 O10 2.607(10) 7 ? Na1 O2 2.718(8) 7 ? Na1 C1 3.014(11) 7 ? Na1 Na1 3.466(3) 7 ? Na1 Na1 3.466(3) 7_545 ? O2 C1 1.291(12) . ? O2 Na1 2.718(8) 7_545 ? O3 C2 1.422(12) 3_655 ? O3 C2 1.422(12) . ? O4 C4 1.394(15) . ? O4 C4 1.394(15) 3_655 ? O5 C3 1.283(13) . ? O7 C3 1.221(14) . ? O7 Na1 2.431(9) 8_574 ? O7 Na1 2.461(10) 2_674 ? O8 Na1 2.542(9) 7_545 ? O10 C1 1.242(13) . ? O10 Na1 2.607(9) 7_545 ? O9 C5 1.469(16) . ? C1 C2 1.490(15) . ? C1 Na1 3.014(11) 7_545 ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.489(18) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 H5A 0.96 . ? C5 H5B 0.96 . ? C5 H5C 0.96 . ? 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 O9 105.8(4) . 3_655 ? O1 V1 O9 105.8(4) . . ? O9 V1 O9 75.9(4) 3_655 . ? O1 V1 O2 94.7(3) . 3_655 ? O9 V1 O2 157.5(3) 3_655 3_655 ? O9 V1 O2 90.0(3) . 3_655 ? O1 V1 O2 94.7(3) . . ? O9 V1 O2 90.0(3) 3_655 . ? O9 V1 O2 157.5(3) . . ? O2 V1 O2 97.5(5) 3_655 . ? O1 V1 O3 163.5(4) . . ? O9 V1 O3 87.1(3) 3_655 . ? O9 V1 O3 87.1(3) . . ? O2 V1 O3 74.7(3) 3_655 . ? O2 V1 O3 74.7(3) . . ? O1 V1 V2 107.9(4) . . ? O9 V1 V2 38.0(2) 3_655 . ? O9 V1 V2 38.0(2) . . ? O2 V1 V2 126.7(2) 3_655 . ? O2 V1 V2 126.7(2) . . ? O3 V1 V2 88.6(3) . . ? O6 V2 O9 105.1(5) . . ? O6 V2 O9 105.1(5) . 3_655 ? O9 V2 O9 75.5(4) . 3_655 ? O6 V2 O5 97.5(4) . 3_655 ? O9 V2 O5 156.2(3) . 3_655 ? O9 V2 O5 91.5(3) 3_655 3_655 ? O6 V2 O5 97.5(4) . . ? O9 V2 O5 91.5(3) . . ? O9 V2 O5 156.2(3) 3_655 . ? O5 V2 O5 93.1(5) 3_655 . ? O6 V2 O4 166.2(6) . . ? O9 V2 O4 85.7(3) . . ? O9 V2 O4 85.7(3) 3_655 . ? O5 V2 O4 73.3(3) 3_655 . ? O5 V2 O4 73.3(3) . . ? O6 V2 V1 106.9(5) . . ? O9 V2 V1 37.8(2) . . ? O9 V2 V1 37.8(2) 3_655 . ? O5 V2 V1 127.5(2) 3_655 . ? O5 V2 V1 127.5(2) . . ? O4 V2 V1 86.9(3) . . ? O10 Na1 O7 166.4(3) . 8_475 ? O10 Na1 O8 85.5(3) . . ? O7 Na1 O8 108.1(3) 8_475 . ? O10 Na1 O7 75.7(3) . 2_675 ? O7 Na1 O7 107.8(5) 8_475 2_675 ? O8 Na1 O7 73.5(3) . 2_675 ? O10 Na1 O8 95.2(3) . 7 ? O7 Na1 O8 72.3(3) 8_475 7 ? O8 Na1 O8 157.7(4) . 7 ? O7 Na1 O8 85.0(3) 2_675 7 ? O10 Na1 O10 100.8(4) . 7 ? O7 Na1 O10 71.9(3) 8_475 7 ? O8 Na1 O10 123.2(3) . 7 ? O7 Na1 O10 163.0(3) 2_675 7 ? O8 Na1 O10 78.7(3) 7 7 ? O10 Na1 O2 96.8(3) . 7 ? O7 Na1 O2 87.1(3) 8_475 7 ? O8 Na1 O2 73.7(3) . 7 ? O7 Na1 O2 146.8(3) 2_675 7 ? O8 Na1 O2 128.1(3) 7 7 ? O10 Na1 O2 49.5(2) 7 7 ? O10 Na1 C1 99.7(3) . 7 ? O7 Na1 C1 78.4(3) 8_475 7 ? O8 Na1 C1 99.1(3) . 7 ? O7 Na1 C1 171.3(3) 2_675 7 ? O8 Na1 C1 102.8(3) 7 7 ? O10 Na1 C1 24.2(3) 7 7 ? O2 Na1 C1 25.4(2) 7 7 ? O10 Na1 Na1 121.7(3) . 7 ? O7 Na1 Na1 45.3(2) 8_475 7 ? O8 Na1 Na1 148.8(3) . 7 ? O7 Na1 Na1 124.7(2) 2_675 7 ? O8 Na1 Na1 44.85(19) 7 7 ? O10 Na1 Na1 42.93(19) 7 7 ? O2 Na1 Na1 87.03(19) 7 7 ? C1 Na1 Na1 63.9(2) 7 7 ? O10 Na1 Na1 48.8(2) . 7_545 ? O7 Na1 Na1 142.2(3) 8_475 7_545 ? O8 Na1 Na1 47.1(2) . 7_545 ? O7 Na1 Na1 44.5(2) 2_675 7_545 ? O8 Na1 Na1 119.0(3) 7 7_545 ? O10 Na1 Na1 143.0(2) 7 7_545 ? O2 Na1 Na1 106.5(2) 7 7_545 ? C1 Na1 Na1 127.0(2) 7 7_545 ? Na1 Na1 Na1 163.6(3) 7 7_545 ? C1 O2 V1 121.9(7) . . ? C1 O2 Na1 90.2(6) . 7_545 ? V1 O2 Na1 143.8(3) . 7_545 ? C2 O3 C2 116.3(11) 3_655 . ? C2 O3 V1 112.1(6) 3_655 . ? C2 O3 V1 112.1(6) . . ? C4 O4 C4 115.3(15) . 3_655 ? C4 O4 V2 109.5(7) . . ? C4 O4 V2 109.5(8) 3_655 . ? C3 O5 V2 124.6(6) . . ? C3 O7 Na1 131.1(7) . 8_574 ? C3 O7 Na1 129.5(7) . 2_674 ? Na1 O7 Na1 90.2(3) 8_574 2_674 ? Na1 O8 Na1 88.0(2) . 7_545 ? C1 O10 Na1 144.8(8) . . ? C1 O10 Na1 96.6(7) . 7_545 ? Na1 O10 Na1 88.3(3) . 7_545 ? C5 O9 V1 126.9(8) . . ? C5 O9 V2 126.5(8) . . ? V1 O9 V2 104.2(3) . . ? O10 C1 O2 123.7(10) . . ? O10 C1 C2 119.5(10) . . ? O2 C1 C2 116.8(9) . . ? O10 C1 Na1 59.2(6) . 7_545 ? O2 C1 Na1 64.4(5) . 7_545 ? C2 C1 Na1 177.9(8) . 7_545 ? O3 C2 C1 111.1(9) . . ? O3 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? O3 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108 . . ? O7 C3 O5 125.3(10) . . ? O7 C3 C4 119.4(10) . . ? O5 C3 C4 115.3(10) . . ? O4 C4 C3 114.2(12) . . ? O4 C4 H4A 108.7 . . ? C3 C4 H4A 108.7 . . ? O4 C4 H4B 108.7 . . ? C3 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? O9 C5 H5A 109.5 . . ? O9 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O9 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? #===END