# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1851 data_General _audit_creation_date 'Sat Nov 20 12:33:34 1999' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' Toshihiro Yamase' _publ_contact_author_address ; Research Laboratory of Resources Utilization Tokyo Institute of Technology 4259 Nagatsuta, Midori-ku, Yokohama 226-8503 Japan ; _publ_contact_author_email ' tyamase@res.titech.ac.jp ' _publ_contact_author_fax ' +81-(0)45-924-5276 ' _publ_contact_author_phone ' +81-(0)45-924-5260 ' _publ_requested_journal ' Dalton Transactions' #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; Crystal and Electronic Structures and Magnetic Susceptibility of the Photochemically Prepared Layered Vanadyl Phosphate, Na(VO)~2~(PO~4~)~2~.4H~2~O ; #_publ_section_title_footnote #; #; loop_ _publ_author_name #_publ_author_footnote _publ_author_address ' Toshihiro Yamase ' ; Research Laboratory of Resources Utilization Tokyo Institute of Technology 4259 Nagatsuta, Midori-ku, Yokohama 226-8503 Japan ; ' Haruyo Makino ' ; Research Laboratory of Resources Utilization Tokyo Institute of Technology 4259 Nagatsuta, Midori-ku, Yokohama 226-8503 Japan ; #------------------------------------------------------------------------------ data_nav2p2 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'H8 Na O14 P2 V2 ' _chemical_formula_moiety '?' _chemical_formula_weight 418.88 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1 ' _symmetry_Int_Tables_number 1 loop_ _symmetry_equiv_pos_as_xyz x,y,z _cell_length_a 6.293(3) _cell_length_b 6.294(3) _cell_length_c 6.844(5) _cell_angle_alpha 107.04(5) _cell_angle_beta 92.34(5) _cell_angle_gamma 90.13(5) _cell_volume 258.9(3) _cell_formula_units_Z 1 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 7.8 _cell_measurement_theta_max 14.8 _cell_measurement_temperature 298 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.020 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.686 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.237 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_process_details '(Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.820 _exptl_absorpt_correction_T_max 1.079 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 1633 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_theta_max 30.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 0.03 #------------------------------------------------------------------------------ # REFINEMENT DATA _reflns_number_total 1633 _reflns_number_gt 948 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.0550 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 948 _refine_ls_number_parameters 89 _refine_ls_goodness_of_fit_ref 1.560 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]' _refine_ls_shift/su_max 0.01 _refine_diff_density_max 0.76 _refine_diff_density_min -0.73 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.300 0.529 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Na' 'Na' 0.036 0.025 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.4100 0.0900 0.0800 0.020(1) Uani 1.00 d . . . V2 V 0.9228(5) 0.6592(5) 0.2675(4) 0.0091(10) Uani 1.00 d . . . P1 P 0.919(2) 0.123(1) 0.164(1) 0.018(2) Uiso 1.00 d . . . P2 P 0.419(1) 0.623(1) 0.172(1) 0.007(1) Uiso 1.00 d . . . Na1 Na 0.753(1) 0.134(1) -0.332(1) 0.043(2) Uani 1.00 d . . . O1 O 0.425(3) 0.156(3) 0.323(3) 0.013(3) Uiso 1.00 d . . . O2 O 0.923(4) 0.582(4) 0.032(4) 0.037(5) Uiso 1.00 d . . . O3 O 0.392(3) 0.391(3) 0.046(3) 0.022(5) Uiso 1.00 d . . . O4 O 0.707(3) 0.097(3) 0.035(3) 0.035(5) Uiso 1.00 d . . . O5 O 0.432(3) 0.764(3) 0.030(3) 0.014(4) Uiso 1.00 d . . . O6 O 0.108(3) 0.056(2) 0.029(3) 0.009(3) Uiso 1.00 d . . . O7 O 0.240(3) 0.687(3) 0.324(3) 0.024(5) Uiso 1.00 d . . . O8 O 0.615(2) 0.657(2) 0.319(2) 0.005(3) Uiso 1.00 d . . . O9 O 0.943(3) 0.367(3) 0.312(3) 0.011(4) Uiso 1.00 d . . . O10 O 0.911(3) 0.976(3) 0.314(3) 0.019(4) Uiso 1.00 d . . . O11 O 0.392(3) -0.001(3) -0.283(3) 0.023(4) Uiso 1.00 d . . . O12 O 0.922(3) -0.234(2) -0.366(3) 0.023(4) Uiso 1.00 d . . . O13 O 1.109(2) 0.307(2) -0.322(2) 0.030(3) Uiso 1.00 d . . . O14 O 0.618(2) 0.493(2) -0.323(2) 0.025(3) Uiso 1.00 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 V1 0.028(3) 0.009(2) 0.024(3) -0.001(2) 0.000(2) 0.007(2) V2 0.004(2) 0.018(2) 0.004(2) 0.000(2) 0.001(1) 0.001(2) Na1 0.046(5) 0.040(5) 0.051(5) 0.013(4) 0.019(4) 0.022(4) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O1 1.59(2) . . yes V1 O4 1.91(2) . . yes V1 O6 1.92(2) . . yes V1 O3 1.98(2) . . yes V1 O5 1.98(2) . 1_545 yes V1 O11 2.38(2) . . yes V1 P1 3.16(1) . 1_455 yes V1 P2 3.181(8) . 1_545 yes V1 P1 3.22(1) . . yes V1 P2 3.228(7) . . yes V1 O7 3.60(2) . 1_545 yes V1 O9 3.61(2) . 1_455 yes V1 O10 3.65(2) . 1_545 yes V1 O8 3.67(1) . . yes V1 NA1 3.692(10) . . yes V1 O10 3.74(2) . 1_445 yes V1 O8 3.77(2) . 1_545 yes V1 O7 3.81(2) . . yes V1 O9 3.84(2) . . yes V1 O13 3.85(1) . 1_455 yes V1 O14 4.20(1) . 1_545 yes V1 O14 4.28(1) . 1_556 yes V1 O12 4.30(2) . 1_455 yes V1 O3 4.34(2) . 1_545 yes V1 O2 4.36(2) . 1_445 yes V1 O5 4.36(2) . . yes V1 O6 4.42(2) . 1_655 yes V1 O13 4.42(1) . 1_456 yes V1 O4 4.42(2) . 1_455 yes V1 NA1 4.425(9) . 1_556 yes V1 O2 4.43(2) . 1_455 yes V1 O14 4.48(1) . . yes V1 O2 4.50(2) . 1_545 yes V1 V2 4.552(3) . 1_445 yes V1 O2 4.56(2) . . yes V1 O11 4.56(2) . 1_556 yes V1 O12 4.59(2) . . yes V1 V2 4.599(3) . 1_545 yes V1 V2 4.643(3) . 1_455 yes V1 V2 4.670(3) . . yes V2 O2 1.54(2) . . yes V2 O10 1.93(2) . . yes V2 O9 1.95(2) . . yes V2 O8 1.98(2) . . yes V2 O7 2.01(2) . 1_655 yes V2 O12 2.40(2) . 1_566 yes V2 P1 3.20(1) . 1_565 yes V2 P2 3.202(10) . . yes V2 P2 3.213(10) . 1_655 yes V2 P1 3.241(9) . . yes V2 O3 3.57(2) . 1_655 yes V2 O6 3.57(2) . 1_665 yes V2 O5 3.59(2) . . yes V2 NA1 3.613(8) . 1_566 yes V2 O4 3.66(2) . . yes V2 O3 3.79(2) . . yes V2 O4 3.79(2) . 1_565 yes V2 O5 3.79(2) . 1_655 yes V2 O14 3.85(1) . 1_556 yes V2 O6 3.87(1) . 1_655 yes V2 O13 4.19(1) . 1_556 yes V2 O13 4.21(1) . . yes V2 O14 4.24(1) . . yes V2 O11 4.26(2) . 1_666 yes V2 O7 4.33(2) . . yes V2 O13 4.35(1) . 1_566 yes V2 O8 4.36(2) . 1_655 yes V2 O1 4.36(2) . 1_665 yes V2 O1 4.38(2) . 1_565 yes V2 O9 4.38(2) . 1_565 yes V2 O10 4.40(2) . 1_545 yes V2 NA1 4.534(8) . . yes V2 O1 4.56(2) . . yes V2 O1 4.56(2) . 1_655 yes V2 O12 4.58(2) . 1_565 yes V2 O11 4.71(2) . 1_566 yes P1 O6 1.52(2) . 1_655 yes P1 O4 1.55(2) . . yes P1 O10 1.57(3) . 1_545 yes P1 O9 1.58(2) . . yes P1 O2 3.25(2) . 1_545 yes P1 O2 3.27(3) . . yes P1 O1 3.31(2) . 1_655 yes P1 O1 3.32(2) . . yes P1 O13 3.52(2) . 1_556 yes P1 NA1 3.53(1) . . yes P1 NA1 3.63(1) . 1_556 yes P1 O3 3.65(2) . 1_655 yes P1 O12 3.67(2) . . yes P1 O5 3.72(2) . 1_545 yes P1 O8 3.77(2) . . yes P1 O7 3.80(2) . 1_645 yes P1 O3 3.89(2) . . yes P1 O8 3.92(2) . 1_545 yes P1 O7 3.93(2) . 1_655 yes P1 O5 3.93(2) . 1_645 yes P1 O13 4.05(2) . . yes P1 O14 4.14(1) . 1_556 yes P1 O11 4.27(2) . 1_655 yes P1 O11 4.33(2) . . yes P1 O12 4.37(2) . 1_566 yes P1 O12 4.43(2) . 1_556 yes P1 P2 4.44(1) . 1_655 yes P1 P2 4.45(1) . . yes P1 P2 4.45(1) . 1_545 yes P1 P2 4.47(1) . 1_645 yes P1 O14 4.70(1) . 1_545 yes P2 O3 1.47(2) . . yes P2 O5 1.50(2) . . yes P2 O8 1.53(2) . . yes P2 O7 1.54(2) . . yes P2 O1 3.20(2) . 1_565 yes P2 O2 3.22(2) . 1_455 yes P2 O2 3.34(3) . . yes P2 O1 3.39(2) . . yes P2 O14 3.52(2) . . yes P2 O4 3.67(2) . . yes P2 O9 3.69(2) . 1_455 yes P2 O6 3.69(2) . 1_565 yes P2 O10 3.73(2) . . yes P2 O11 3.79(2) . 1_566 yes P2 O13 3.84(1) . 1_455 yes P2 O4 3.85(2) . 1_565 yes P2 O9 3.87(2) . . yes P2 O10 3.89(2) . 1_455 yes P2 O6 3.92(2) . . yes P2 O14 3.94(2) . 1_556 yes P2 O11 4.24(2) . . yes P2 O12 4.28(2) . 1_566 yes P2 NA1 4.39(1) . 1_566 yes P2 O11 4.43(2) . 1_565 yes P2 O12 4.44(2) . 1_466 yes P2 NA1 4.49(1) . . yes NA1 O14 2.40(2) . . yes NA1 O13 2.48(2) . . yes NA1 O11 2.49(2) . . yes NA1 O12 2.51(2) . . yes NA1 O10 2.58(2) . 1_544 yes NA1 O4 2.61(2) . . yes NA1 O1 3.11(2) . 1_554 yes NA1 O2 3.31(2) . . yes NA1 O8 3.33(1) . 1_544 yes NA1 O6 3.40(2) . 1_655 yes NA1 O9 3.44(2) . 1_554 yes NA1 O3 3.53(2) . . yes NA1 O11 4.13(2) . 1_655 yes NA1 O14 4.14(2) . 1_545 yes NA1 O12 4.19(2) . 1_565 yes NA1 O13 4.20(2) . 1_455 yes NA1 O4 4.27(2) . 1_554 yes NA1 O9 4.33(2) . . yes NA1 O7 4.40(2) . 1_544 yes NA1 O5 4.40(2) . 1_545 yes NA1 O7 4.43(2) . 1_644 yes NA1 O5 4.54(2) . . yes NA1 O8 4.66(2) . 1_554 yes NA1 O5 4.68(2) . 1_544 yes NA1 O3 4.71(2) . 1_655 yes O1 O4 2.65(3) . . yes O1 O5 2.69(2) . 1_545 yes O1 O6 2.71(2) . . yes O1 O3 2.73(3) . . yes O1 O14 2.93(2) . 1_556 yes O1 O13 3.13(2) . 1_456 yes O1 O11 3.14(3) . 1_556 yes O1 O7 3.17(3) . 1_545 yes O1 O10 3.26(3) . 1_545 yes O1 O9 3.33(2) . 1_455 yes O1 O8 3.36(2) . 1_545 yes O1 O8 3.38(2) . . yes O1 O10 3.41(3) . 1_445 yes O1 O9 3.53(3) . . yes O1 O7 3.54(3) . . yes O1 O11 3.97(3) . . yes O1 O3 4.63(2) . 1_545 yes O1 O2 4.71(3) . 1_445 yes O2 O9 2.65(3) . . yes O2 O10 2.66(3) . . yes O2 O7 2.70(3) . 1_655 yes O2 O8 2.76(3) . . yes O2 O13 2.83(2) . . yes O2 O14 2.95(3) . . yes O2 O3 3.20(3) . 1_655 yes O2 O6 3.20(3) . 1_665 yes O2 O12 3.26(3) . 1_565 yes O2 O5 3.30(3) . . yes O2 O4 3.35(3) . . yes O2 O5 3.40(3) . 1_655 yes O2 O6 3.51(3) . 1_655 yes O2 O4 3.51(3) . 1_565 yes O2 O3 3.56(3) . . yes O2 O12 3.94(3) . 1_566 yes O2 O8 4.67(3) . 1_655 yes O2 O9 4.72(3) . 1_554 yes O3 O5 2.39(3) . . yes O3 O7 2.47(3) . . yes O3 O8 2.49(2) . . yes O3 O4 2.70(3) . . yes O3 O6 2.74(3) . . yes O3 O11 2.81(2) . . yes O3 O13 2.94(2) . 1_455 yes O3 O14 3.16(3) . . yes O3 O9 3.45(3) . 1_455 yes O3 O9 3.87(3) . . yes O3 O5 3.93(3) . 1_545 yes O3 O14 4.36(2) . 1_556 yes O3 O6 4.58(3) . 1_565 yes O3 O4 4.68(3) . 1_455 yes O4 O6 2.54(3) . 1_655 yes O4 O10 2.55(3) . 1_545 yes O4 O9 2.56(2) . . yes O4 O5 2.71(3) . 1_545 yes O4 O11 2.81(3) . . yes O4 O12 3.27(2) . . yes O4 O8 3.55(2) . . yes O4 O6 3.78(3) . . yes O4 O8 3.88(3) . 1_545 yes O4 O14 3.90(2) . 1_545 yes O4 O14 4.00(3) . . yes O4 O13 4.06(3) . . yes O4 O14 4.43(2) . 1_556 yes O4 O5 4.55(3) . . yes O5 O8 2.51(3) . . yes O5 O7 2.55(3) . . yes O5 O6 2.75(3) . 1_565 yes O5 O14 2.82(2) . . yes O5 O11 2.94(3) . 1_565 yes O5 O10 3.56(3) . . yes O5 O13 3.70(2) . 1_455 yes O5 O10 3.91(3) . 1_455 yes O5 O12 4.11(3) . 1_465 yes O5 O12 4.19(3) . 1_565 yes O5 O11 4.51(3) . 1_566 yes O5 O6 4.63(3) . 1_665 yes O5 O11 4.66(2) . . yes O6 O10 2.52(3) . 1_445 yes O6 O9 2.57(2) . 1_455 yes O6 O11 2.79(3) . . yes O6 O12 2.98(2) . 1_455 yes O6 O13 3.24(2) . 1_455 yes O6 O7 3.57(3) . 1_545 yes O6 O7 3.96(2) . . yes O6 O13 4.25(2) . 1_456 yes O6 O13 4.62(2) . 1_445 yes O6 O14 4.71(2) . 1_445 yes O7 O8 2.37(3) . . yes O7 O9 2.73(3) . 1_455 yes O7 O10 2.77(3) . 1_455 yes O7 O12 2.91(3) . 1_466 yes O7 O11 2.95(2) . 1_566 yes O7 O14 3.78(3) . 1_556 yes O7 O8 3.93(3) . 1_455 yes O7 O13 3.98(3) . 1_456 yes O7 O13 4.05(2) . 1_466 yes O7 O13 4.41(2) . 1_455 yes O7 O10 4.61(3) . . yes O7 O12 4.67(3) . 1_566 yes O7 O9 4.70(3) . 1_465 yes O8 O9 2.74(2) . . yes O8 O10 2.75(3) . . yes O8 O12 2.76(2) . 1_566 yes O8 O14 2.93(2) . 1_556 yes O8 O11 3.30(2) . 1_566 yes O8 O14 4.21(2) . . yes O8 O9 4.60(2) . 1_455 yes O8 O10 4.66(2) . 1_545 yes O9 O10 2.47(3) . 1_545 yes O9 O13 2.80(2) . 1_556 yes O9 O12 2.82(2) . 1_566 yes O9 O14 3.21(2) . 1_556 yes O9 O10 3.84(3) . . yes O9 O13 4.41(2) . . yes O10 O12 2.87(3) . 1_566 yes O10 O13 2.96(2) . 1_566 yes O10 O14 3.98(2) . 1_566 yes O10 O11 3.98(3) . 1_666 yes O10 O11 4.34(3) . 1_566 yes O10 O12 4.45(3) . 1_565 yes O11 O13 2.70(2) . 1_455 yes O11 O12 3.25(2) . 1_455 yes O11 O14 3.44(2) . 1_545 yes O11 O14 3.49(2) . . yes O11 O12 3.65(2) . . yes O11 O13 4.63(2) . 1_445 yes O12 O14 2.66(2) . 1_545 yes O12 O13 3.21(2) . 1_545 yes O12 O13 3.53(2) . . yes O13 O14 3.31(2) . . yes O13 O14 3.40(2) . 1_655 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 V1 O4 98.1(9) 1_555 1_555 1_555 yes O1 V1 O6 100.7(8) 1_555 1_555 1_555 yes O1 V1 O3 99.2(8) 1_555 1_555 1_555 yes O1 V1 O5 96.8(9) 1_555 1_555 1_545 yes O1 V1 O11 178.6(7) 1_555 1_555 1_555 yes O4 V1 O6 161.1(8) 1_555 1_555 1_555 yes O4 V1 O3 88.0(9) 1_555 1_555 1_555 yes O4 V1 O5 88.1(8) 1_555 1_555 1_545 yes O4 V1 O11 81.1(7) 1_555 1_555 1_555 yes O6 V1 O3 89.2(8) 1_555 1_555 1_555 yes O6 V1 O5 89.4(7) 1_555 1_555 1_545 yes O6 V1 O11 80.0(7) 1_555 1_555 1_555 yes O3 V1 O5 163.9(8) 1_555 1_555 1_545 yes O3 V1 O11 79.7(7) 1_555 1_555 1_555 yes O5 V1 O11 84.3(7) 1_545 1_555 1_555 yes O2 V2 O10 99(1) 1_555 1_555 1_555 yes O2 V2 O9 97(1) 1_555 1_555 1_555 yes O2 V2 O8 102.3(10) 1_555 1_555 1_555 yes O2 V2 O7 97(1) 1_555 1_555 1_655 yes O2 V2 O12 178.0(10) 1_555 1_555 1_566 yes O10 V2 O9 162.4(8) 1_555 1_555 1_555 yes O10 V2 O8 89.3(7) 1_555 1_555 1_555 yes O10 V2 O7 89.2(8) 1_555 1_555 1_655 yes O10 V2 O12 82.4(8) 1_555 1_555 1_566 yes O9 V2 O8 88.5(7) 1_555 1_555 1_555 yes O9 V2 O7 86.8(8) 1_555 1_555 1_655 yes O9 V2 O12 80.1(6) 1_555 1_555 1_566 yes O8 V2 O7 159.6(7) 1_555 1_555 1_655 yes O8 V2 O12 77.5(6) 1_555 1_555 1_566 yes O7 V2 O12 82.1(7) 1_655 1_555 1_566 yes O6 P1 O4 111(1) 1_655 1_555 1_555 yes O6 P1 O10 109(1) 1_655 1_555 1_545 yes O6 P1 O9 112(1) 1_655 1_555 1_555 yes O6 P1 O2 74.5(8) 1_655 1_555 1_545 yes O6 P1 O2 86.0(8) 1_655 1_555 1_555 yes O4 P1 O10 110(1) 1_555 1_555 1_545 yes O4 P1 O9 109(1) 1_555 1_555 1_555 yes O4 P1 O2 86.3(8) 1_555 1_555 1_545 yes O4 P1 O2 79.1(9) 1_555 1_555 1_555 yes O10 P1 O9 103(1) 1_545 1_555 1_555 yes O10 P1 O2 54.3(8) 1_545 1_555 1_545 yes O10 P1 O2 156.4(9) 1_545 1_555 1_555 yes O9 P1 O2 156(1) 1_555 1_555 1_545 yes O9 P1 O2 53.2(9) 1_555 1_555 1_555 yes O2 P1 O2 149.3(9) 1_545 1_555 1_555 yes O3 P2 O5 107(1) 1_555 1_555 1_555 yes O3 P2 O8 112(1) 1_555 1_555 1_555 yes O3 P2 O7 110(1) 1_555 1_555 1_555 yes O3 P2 O1 162(1) 1_555 1_555 1_565 yes O3 P2 O2 76.0(10) 1_555 1_555 1_455 yes O5 P2 O8 111(1) 1_555 1_555 1_555 yes O5 P2 O7 114(1) 1_555 1_555 1_555 yes O5 P2 O1 56.6(8) 1_555 1_555 1_565 yes O5 P2 O2 83.7(10) 1_555 1_555 1_455 yes O8 P2 O7 101(1) 1_555 1_555 1_555 yes O8 P2 O1 82.1(6) 1_555 1_555 1_565 yes O8 P2 O2 157.6(9) 1_555 1_555 1_455 yes O7 P2 O1 74.8(8) 1_555 1_555 1_565 yes O7 P2 O2 56.8(9) 1_555 1_555 1_455 yes O1 P2 O2 94.4(5) 1_565 1_555 1_455 yes O14 NA1 O13 85.5(5) 1_555 1_555 1_555 yes O14 NA1 O11 91.3(6) 1_555 1_555 1_555 yes O14 NA1 O12 174.0(7) 1_555 1_555 1_555 yes O14 NA1 O10 106.1(7) 1_555 1_555 1_544 yes O14 NA1 O4 105.6(6) 1_555 1_555 1_555 yes O14 NA1 O1 62.7(5) 1_555 1_555 1_554 yes O13 NA1 O11 170.8(6) 1_555 1_555 1_555 yes O13 NA1 O12 90.0(6) 1_555 1_555 1_555 yes O13 NA1 O10 71.7(6) 1_555 1_555 1_544 yes O13 NA1 O4 105.8(6) 1_555 1_555 1_555 yes O13 NA1 O1 118.3(6) 1_555 1_555 1_554 yes O11 NA1 O12 93.8(6) 1_555 1_555 1_555 yes O11 NA1 O10 117.5(6) 1_555 1_555 1_544 yes O11 NA1 O4 66.8(7) 1_555 1_555 1_555 yes O11 NA1 O1 67.2(6) 1_555 1_555 1_554 yes O12 NA1 O10 68.7(7) 1_555 1_555 1_544 yes O12 NA1 O4 79.3(7) 1_555 1_555 1_555 yes O12 NA1 O1 116.5(5) 1_555 1_555 1_554 yes O10 NA1 O4 147.8(8) 1_544 1_555 1_555 yes O10 NA1 O1 69.3(6) 1_544 1_555 1_554 yes O4 NA1 O1 132.1(7) 1_555 1_555 1_554 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag V1 V2 4.552(3) . 1_445 yes V1 V2 4.599(3) . 1_545 yes V1 V2 4.643(3) . 1_455 yes V1 V2 4.670(3) . . yes #------------------------------------------------------------------------------ # NOTE - the following data is from a solution of the same structure in P-1 # The inferior final solution in this space group demonstrates that P1 is the # better solution #------------------------------------------------------------------------------ data_P-1 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'H8 Na O14 P2 V2 ' _chemical_formula_moiety '?' _chemical_formula_weight 418.88 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z _cell_length_a 6.293(3) _cell_length_b 6.294(3) _cell_length_c 6.844(5) _cell_angle_alpha 107.04(5) _cell_angle_beta 92.34(5) _cell_angle_gamma 90.13(5) _cell_volume 258.9(3) _cell_formula_units_Z 1 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 7.8 _cell_measurement_theta_max 14.8 _cell_measurement_temperature 298 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.020 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.686 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.237 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_process_details '(Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.820 _exptl_absorpt_correction_T_max 1.079 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 1633 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_theta_max 30.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 0.03 #------------------------------------------------------------------------------ # REFINEMENT DATA _reflns_number_total 1633 _reflns_number_gt 948 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.0720 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 948 _refine_ls_number_parameters 100 _refine_ls_goodness_of_fit_ref 2.06 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]' _refine_ls_shift/su_max 0.0015 _refine_diff_density_max 0.88 _refine_diff_density_min -0.81 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.300 0.529 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Na' 'Na' 0.036 0.025 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.7564(3) 0.7844(3) 0.5937(3) 0.0141(4) Uani 1.00 d . . . P1 P 0.2507(4) 0.7504(4) 0.5038(4) 0.0124(6) Uani 1.00 d . . . Na1 Na 0.413(2) 0.737(2) 1.004(2) 0.040(3) Uani 0.50 d P . . O2 O 0.748(1) 0.713(1) 0.353(1) 0.028(2) Uani 1.00 d . . . O5 O 0.262(1) 0.894(1) 0.3576(9) 0.017(2) Uani 1.00 d . . . O6 O 1.0656(10) 0.818(1) 0.6479(9) 0.016(2) Uani 1.00 d . . . O8 O 0.452(1) 0.780(1) 0.6430(10) 0.018(2) Uani 1.00 d . . . O9 O 0.776(1) 0.492(1) 0.6342(10) 0.017(2) Uani 1.00 d . . . O11 O 0.765(1) 0.885(1) 0.959(1) 0.024(2) Uani 1.00 d . . . O12 O 0.058(2) 0.557(3) 0.997(2) 0.031(5) Uani 0.50 d P . . O13 O 0.547(3) 0.373(2) 0.995(2) 0.023(4) Uani 0.50 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 V1 0.0146(9) 0.0142(8) 0.0133(9) 0.0002(7) 0.0009(6) 0.0039(7) P1 0.011(1) 0.011(1) 0.015(1) -0.0004(10) -0.001(1) 0.004(1) Na1 0.041(7) 0.025(6) 0.063(8) 0.012(5) 0.019(5) 0.024(6) O2 0.032(5) 0.038(5) 0.013(4) -0.001(4) 0.003(3) 0.004(3) O5 0.022(4) 0.019(3) 0.010(3) 0.001(3) 0.002(3) 0.004(3) O6 0.015(3) 0.016(3) 0.018(4) 0.000(3) 0.004(3) 0.005(3) O8 0.017(3) 0.020(3) 0.015(4) 0.001(3) -0.002(3) 0.001(3) O9 0.021(4) 0.013(3) 0.016(4) 0.000(3) -0.001(3) 0.002(3) O11 0.028(4) 0.023(4) 0.021(4) -0.004(3) 0.003(3) 0.007(3) O12 0.03(1) 0.04(1) 0.020(8) 0.008(7) 0.001(8) 0.008(8) O13 0.033(10) 0.014(8) 0.026(9) -0.005(7) 0.003(7) 0.013(7) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O2 1.576(7) . . yes V1 O9 1.944(7) . . yes V1 O5 1.958(7) . 2_676 yes V1 O8 1.958(7) . . yes V1 O6 1.965(7) . . yes V1 O11 2.389(7) . . yes V1 O6 3.581(8) . 2_776 yes V1 O9 3.596(7) . 2_766 yes V1 O5 3.611(7) . . yes V1 O8 3.659(6) . 2_666 yes V1 O5 3.775(7) . 1_655 yes V1 O8 3.784(8) . 2_676 yes V1 O13 3.82(2) . 2_667 yes V1 O9 3.824(6) . 2_666 yes V1 O6 3.854(6) . 2_766 yes V1 O12 3.89(2) . 1_655 yes V1 O12 4.14(2) . 2_667 yes V1 O13 4.17(1) . 1_565 yes V1 O12 4.20(2) . 2_666 yes V1 O13 4.23(2) . 2_666 yes V1 O11 4.273(7) . 2_777 yes V1 O13 4.31(1) . 1_554 yes V1 O2 4.364(8) . 2_776 yes V1 O6 4.379(7) . 1_455 yes V1 O8 4.379(7) . 1_655 yes V1 O5 4.380(7) . 2_666 yes V1 O9 4.380(7) . 1_565 yes V1 O12 4.40(1) . 2_677 yes V1 O12 4.42(2) . 1_654 yes V1 O2 4.433(8) . 2_676 yes V1 O2 4.507(8) . 2_766 yes V1 O13 4.52(2) . . yes V1 O2 4.554(8) . 2_666 yes V1 O11 4.575(8) . 1_554 yes V1 O11 4.646(7) . 2_677 yes P1 O8 1.532(7) . . yes P1 O5 1.535(8) . . yes P1 O6 1.537(7) . 1_455 yes P1 O9 1.544(6) . 2_666 yes P1 O2 3.226(8) . 2_676 yes P1 O2 3.276(8) . 1_455 yes P1 O2 3.322(8) . . yes P1 O2 3.342(9) . 2_666 yes P1 O12 3.49(2) . 1_554 yes P1 O13 3.56(2) . 2_666 yes P1 O9 3.665(7) . 1_455 yes P1 O5 3.717(7) . 2_676 yes P1 O8 3.722(7) . 2_666 yes P1 O11 3.726(7) . 2_677 yes P1 O6 3.733(7) . 2_676 yes P1 O12 3.85(1) . 2_566 yes P1 O9 3.872(7) . . yes P1 O8 3.887(8) . 2_676 yes P1 O13 3.90(2) . 2_667 yes P1 O5 3.917(7) . 2_576 yes P1 O6 3.931(7) . 2_666 yes P1 O13 4.11(1) . 1_554 yes P1 O12 4.13(2) . . yes P1 O11 4.301(7) . . yes P1 O11 4.312(6) . 2_666 yes P1 O11 4.359(8) . 1_455 yes P1 O11 4.417(8) . 2_676 yes P1 O13 4.68(1) . 1_565 yes NA1 O13 0.74(2) . 2_667 yes NA1 O13 2.43(2) . . yes NA1 O11 2.47(1) . . yes NA1 O12 2.50(2) . . yes NA1 O5 2.56(1) . 1_556 yes NA1 O11 2.58(1) . 2_677 yes NA1 O8 2.58(1) . . yes NA1 O2 3.16(1) . 1_556 yes NA1 O2 3.28(1) . 2_666 yes NA1 O6 3.35(1) . 1_455 yes NA1 O8 3.37(1) . 2_677 yes NA1 O9 3.46(1) . 2_667 yes NA1 O12 3.49(2) . 2_567 yes NA1 O9 3.49(1) . . yes NA1 O12 3.81(2) . 2_667 yes NA1 O13 4.11(2) . 1_565 yes NA1 O11 4.15(1) . 2_667 yes NA1 O11 4.20(1) . 1_455 yes NA1 O12 4.22(2) . 1_655 yes NA1 O9 4.29(1) . 2_666 yes NA1 O8 4.30(1) . 1_556 yes NA1 O6 4.39(1) . 2_677 yes NA1 O5 4.41(1) . 2_676 yes NA1 O6 4.44(1) . 2_777 yes NA1 O5 4.56(1) . 2_666 yes NA1 O8 4.65(1) . 2_667 yes NA1 O9 4.66(1) . 1_455 yes NA1 O5 4.69(1) . 2_677 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 V1 O9 99.1(4) 1_555 1_555 1_555 yes O2 V1 O5 98.1(4) 1_555 1_555 2_676 yes O2 V1 O8 100.1(3) 1_555 1_555 1_555 yes O2 V1 O6 99.8(3) 1_555 1_555 1_555 yes O2 V1 O11 178.8(4) 1_555 1_555 1_555 yes O9 V1 O5 162.8(3) 1_555 1_555 2_676 yes O9 V1 O8 88.3(3) 1_555 1_555 1_555 yes O9 V1 O6 88.2(3) 1_555 1_555 1_555 yes O9 V1 O11 80.0(3) 1_555 1_555 1_555 yes O5 V1 O8 88.4(3) 2_676 1_555 1_555 yes O5 V1 O6 89.2(3) 2_676 1_555 1_555 yes O5 V1 O11 82.9(3) 2_676 1_555 1_555 yes O8 V1 O6 160.1(3) 1_555 1_555 1_555 yes O8 V1 O11 79.2(3) 1_555 1_555 1_555 yes O6 V1 O11 80.9(3) 1_555 1_555 1_555 yes O8 P1 O5 111.2(4) 1_555 1_555 1_555 yes O8 P1 O6 105.7(4) 1_555 1_555 1_455 yes O8 P1 O9 111.2(4) 1_555 1_555 2_666 yes O8 P1 O2 84.0(3) 1_555 1_555 2_676 yes O8 P1 O2 160.9(3) 1_555 1_555 1_455 yes O5 P1 O6 111.6(4) 1_555 1_555 1_455 yes O5 P1 O9 105.7(4) 1_555 1_555 2_666 yes O5 P1 O2 55.7(3) 1_555 1_555 2_676 yes O5 P1 O2 82.0(3) 1_555 1_555 1_455 yes O6 P1 O9 111.5(4) 1_455 1_555 2_666 yes O6 P1 O2 74.2(3) 1_455 1_555 2_676 yes O6 P1 O2 55.6(3) 1_455 1_555 1_455 yes O9 P1 O2 160.3(3) 2_666 1_555 2_676 yes O9 P1 O2 76.4(3) 2_666 1_555 1_455 yes O2 P1 O2 93.2(2) 2_676 1_555 1_455 yes O13 NA1 O13 1(1) 2_667 1_555 1_555 yes O13 NA1 O11 94(1) 2_667 1_555 1_555 yes O13 NA1 O12 83(1) 2_667 1_555 1_555 yes O13 NA1 O5 103(1) 2_667 1_555 1_556 yes O13 NA1 O11 171(1) 2_667 1_555 2_677 yes O13 NA1 O8 108(1) 2_667 1_555 1_555 yes O13 NA1 O2 61(1) 2_667 1_555 1_556 yes O13 NA1 O2 59(1) 2_667 1_555 2_666 yes O13 NA1 O11 93.9(6) 1_555 1_555 1_555 yes O13 NA1 O12 83.8(6) 1_555 1_555 1_555 yes O13 NA1 O5 105.5(6) 1_555 1_555 1_556 yes O13 NA1 O11 173.0(7) 1_555 1_555 2_677 yes O13 NA1 O8 107.0(6) 1_555 1_555 1_555 yes O13 NA1 O2 62.7(5) 1_555 1_555 1_556 yes O13 NA1 O2 58.3(4) 1_555 1_555 2_666 yes O11 NA1 O12 171.9(6) 1_555 1_555 1_555 yes O11 NA1 O5 115.7(4) 1_555 1_555 1_556 yes O11 NA1 O11 92.2(4) 1_555 1_555 2_677 yes O11 NA1 O8 67.0(4) 1_555 1_555 1_555 yes O11 NA1 O2 67.8(3) 1_555 1_555 1_556 yes O11 NA1 O2 115.6(4) 1_555 1_555 2_666 yes O12 NA1 O5 72.4(5) 1_555 1_555 1_556 yes O12 NA1 O11 90.6(5) 1_555 1_555 2_677 yes O12 NA1 O8 106.1(6) 1_555 1_555 1_555 yes O12 NA1 O2 117.5(6) 1_555 1_555 1_556 yes O12 NA1 O2 56.6(4) 1_555 1_555 2_666 yes O5 NA1 O11 68.6(3) 1_556 1_555 2_677 yes O5 NA1 O8 147.2(5) 1_556 1_555 1_555 yes O5 NA1 O2 68.7(3) 1_556 1_555 1_556 yes O5 NA1 O2 126.9(5) 1_556 1_555 2_666 yes O11 NA1 O8 78.7(4) 2_677 1_555 1_555 yes O11 NA1 O2 116.8(4) 2_677 1_555 1_556 yes O11 NA1 O2 121.6(4) 2_677 1_555 2_666 yes O8 NA1 O2 132.6(5) 1_555 1_555 1_556 yes O8 NA1 O2 68.7(3) 1_555 1_555 2_666 yes O2 NA1 O2 121.0(4) 1_556 1_555 2_666 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag V1 V1 4.553(4) . 2_776 yes V1 V1 4.601(4) . 2_676 yes V1 V1 4.641(4) . 2_766 yes V1 V1 4.668(4) . 2_666 yes #------------------------------------------------------------------------------