# 2. SUBMISSION DETAILS _publ_contact_author_name 'Shpanchenko R.V.' _publ_contact_author_address ; Chemistry Department, Moscow State University, Moscow 119992, Russia ; _publ_contact_author_email shpanchenko@icr.chem.msu.ru _publ_contact_author_fax '7(095)9394788' _publ_contact_author_phone '7(095)9393490' _publ_requested_journal '' _publ_requested_category ? _publ_contact_letter ; ? ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Crystal Structure, Polymorphism and Properties of the New Vanadylphosphate Na4VO(PO4)2 ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Rodion V. Panin' # name ; ? # footnote ; ;Department of Chemistry Moscow State University 119992 Moscow, Russia # address ; 'Roman V. Shpanchenko' # name ;corresponding author # footnote ; ;Department of Chemistry Moscow State University 119992 Moscow, Russia # address ; 'Andrey V. Mironov' # name ; ? # footnote ; ;Department of Chemistry Moscow State University 119992 Moscow, Russia # address ; 'Yuri A. Velikodny' # name ; ? # footnote ; ;Department of Chemistry Moscow State University 119992 Moscow, Russia # address ; 'Evgeny V. Antipov' # name ; ? # footnote ; ;Department of Chemistry Moscow State University 119992 Moscow, Russia # address ; 'Joke Hadermann' # name ; ? # footnote ; ;EMAT University of Antwerp (RUCA) Groenenborgerlaan 171 2020 Antwerp Belgium # address ; 'Vasily A. Tarnopolsky' # name ; ? # footnote ; ;Kurnakov Institute of General and Inorganic Chemistry RAS Leninsky pr. 31 Moscow 119991 Russia # address ; 'Andrey B. Yaroslavtsev' # name ; ? # footnote ; ;Kurnakov Institute of General and Inorganic Chemistry RAS Leninsky pr. 31 Moscow 119991 Russia # address ; #======================================================================= # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_introduction ; ? ; _publ_section_experimental ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_exptl_solution ; ? ; _publ_section_discussion ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; Akselrud L.G., Gryn Yu.N., Zavalij P.U., Pecharsky V.K., Fundamensky V.S. (1989), ECM-12, Moscow, USSR, 155. Becker, P. J. & Coppens, P. (1974). Acta Cryst. A30, 129-153. Pet\3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_gt 0.0405 _refine_ls_R_factor_all 0.0294 _refine_ls_wR_factor_ref 0.0405 _refine_ls_goodness_of_fit_ref 1.71 _refine_ls_goodness_of_fit_gt 1.71 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 2520 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0017 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_max 0.79 _refine_diff_density_min -0.67 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 0.059211 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_versus_stol_list Na 0.036 0.025 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 11.000 10.568 9.760 9.027 8.335 7.618 6.881 6.156 5.471 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 4.848 4.293 3.811 3.398 3.048 2.754 2.509 2.305 2.137 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 1.997 1.881 1.784 1.703 1.634 1.575 1.524 1.479 1.438 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 1.401 1.367 1.334 1.304 1.275 1.247 1.219 1.191 1.164 ; V 0.301 0.529 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 23.000 22.208 20.474 18.661 17.003 15.465 14.026 12.705 11.530 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 10.515 9.660 8.952 8.373 7.898 7.506 7.178 6.892 6.640 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 6.406 6.187 5.972 5.762 5.553 5.346 5.139 4.933 4.730 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 4.529 4.333 4.142 3.956 3.777 3.604 3.438 3.281 3.133 ; P 0.102 0.094 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 15.000 14.458 13.138 11.629 10.327 9.335 8.600 8.029 7.547 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 7.103 6.674 6.250 5.829 5.418 5.020 4.640 4.284 3.953 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 3.649 3.372 3.122 2.898 2.698 2.521 2.364 2.226 2.104 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 1.997 1.903 1.820 1.747 1.683 1.626 1.575 1.530 1.490 ; O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 8.000 7.798 7.245 6.472 5.623 4.808 4.089 3.489 3.006 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 2.629 2.338 2.115 1.946 1.816 1.714 1.635 1.568 1.512 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 1.463 1.419 1.377 1.337 1.298 1.259 1.221 1.183 1.145 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 1.107 1.070 1.033 0.997 0.961 0.926 0.891 0.857 0.824 ; _computing_data_collection 'CAD4 Users Manual (Enraf-Nonius, 1988)' _computing_cell_refinement 'CAD4 Users Manual (Enraf-Nonius, 1988)' _computing_data_reduction '(Jana2000; Petricek and Dusek, 2000)' _computing_structure_solution 'CSD (Akselrud et al., 1989)' _computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)' _computing_molecular_graphics ? _computing_publication_material '(Jana2000; Petricek and Dusek, 2000)' #======================================================================= # 9. 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_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.733825(19) 0.24046(2) 0.71882(4) Uani 0.00654(7) 8 1 d . . . P1 P 0.37241(3) 0.13897(3) 0.50111(7) Uani 0.00719(11) 8 1 d . . . P2 P 0.11951(3) 0.10868(3) 0.49849(7) Uani 0.00650(11) 8 1 d . . . Na1 Na 0.88239(5) 0.13791(6) 0.49664(12) Uani 0.0139(2) 8 1 d . . . Na2 Na 0.52511(6) 0.24540(6) 0.25623(11) Uani 0.0165(2) 8 1 d . . . Na3 Na 0.49538(6) 0.99419(6) 0.26968(14) Uani 0.0200(3) 8 1 d . . . Na4 Na 0.72534(6) 0.02381(7) 0.31389(15) Uani 0.0276(3) 8 1 d . . . O1 O 0.02405(8) 0.10267(10) 0.49132(19) Uani 0.0132(4) 8 1 d . . . O2 O 0.31685(9) 0.15150(10) 0.68029(18) Uani 0.0121(4) 8 1 d . . . O3 O 0.31941(9) 0.15884(10) 0.31916(19) Uani 0.0119(3) 8 1 d . . . O4 O 0.40109(10) 0.03937(11) 0.4998(2) Uani 0.0167(4) 8 1 d . . . O5 O 0.15989(9) 0.01397(10) 0.4957(2) Uani 0.0132(4) 8 1 d . . . O6 O 0.14266(9) 0.16382(10) 0.67933(19) Uani 0.0109(3) 8 1 d . . . O7 O 0.14765(8) 0.16353(10) 0.31989(18) Uani 0.0100(3) 8 1 d . . . O8 O 0.73830(8) 0.20007(10) 0.50109(17) Uani 0.0093(3) 8 1 d . . . O9 O 0.44440(10) 0.20707(12) 0.5086(2) Uani 0.0192(4) 8 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _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 V 0.00665(13) 0.00802(12) 0.00496(12) 0.00019(10) 0.00008(9) 0.00080(10) P1 P 0.00642(19) 0.00924(19) 0.00591(19) 0.00152(14) 0.00022(15) -0.00004(15) P2 P 0.00625(18) 0.00676(18) 0.00650(19) -0.00087(14) -0.00021(15) -0.00007(15) Na1 Na 0.0109(3) 0.0134(4) 0.0174(4) 0.0003(3) 0.0001(3) 0.0002(3) Na2 Na 0.0111(4) 0.0232(4) 0.0152(4) -0.0001(3) 0.0003(3) -0.0007(3) Na3 Na 0.0220(5) 0.0240(4) 0.0139(4) 0.0062(4) -0.0006(3) -0.0026(4) Na4 Na 0.0264(5) 0.0280(5) 0.0283(6) -0.0075(4) -0.0143(4) 0.0117(4) O1 O 0.0071(5) 0.0168(7) 0.0157(7) -0.0022(5) -0.0002(5) 0.0000(5) O2 O 0.0131(6) 0.0152(6) 0.0080(6) 0.0048(5) 0.0027(5) 0.0007(5) O3 O 0.0124(6) 0.0156(6) 0.0077(6) 0.0057(5) -0.0018(4) -0.0002(5) O4 O 0.0215(7) 0.0151(7) 0.0133(6) 0.0089(6) 0.0020(6) 0.0012(5) O5 O 0.0157(6) 0.0096(6) 0.0144(6) 0.0019(5) -0.0010(5) -0.0003(5) O6 O 0.0118(6) 0.0124(6) 0.0085(6) -0.0036(5) -0.0003(5) -0.0028(4) O7 O 0.0111(6) 0.0112(6) 0.0076(6) -0.0036(5) -0.0003(4) 0.0019(4) O8 O 0.0116(6) 0.0111(6) 0.0052(5) 0.0003(5) 0.0000(5) 0.0000(4) O9 O 0.0137(6) 0.0256(8) 0.0183(8) -0.0083(6) 0.0002(6) -0.0011(6) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag V1 O2 . 2_556 1.9837(14) yes V1 O3 . 7_556 2.0208(15) yes V1 O6 . 2_556 1.9694(14) yes V1 O7 . 7_556 1.9794(14) yes V1 O8 . . 1.6392(12) yes V1 O8 . 8_555 2.1633(13) yes P1 O2 . . 1.5517(14) yes P1 O3 . . 1.5607(14) yes P1 O4 . . 1.5166(16) yes P1 O9 . . 1.5190(17) yes P2 O1 . . 1.5314(14) yes P2 O5 . . 1.5190(15) yes P2 O6 . . 1.5462(14) yes P2 O7 . . 1.5524(14) yes Na1 O1 . 1_655 2.3248(16) yes Na1 O2 . 2_556 2.5075(16) yes Na1 O3 . 2_555 2.4551(16) yes Na1 O5 . 5_656 2.3063(17) yes Na1 O8 . . 2.4768(16) yes Na1 O9 . 7_556 2.459(2) yes Na2 O1 . 2_555 2.7044(17) yes Na2 O1 . 7_556 2.8294(17) yes Na2 O6 . 7_556 2.3411(16) yes Na2 O7 . 2_555 2.3548(16) yes Na2 O9 . . 2.2629(17) yes Na2 O9 . 8_554 2.2735(17) yes Na3 O1 . 2_565 2.4595(17) yes Na3 O1 . 6_564 2.4279(17) yes Na3 O4 . 1_565 2.3065(18) yes Na3 O4 . 5_666 2.3674(18) yes Na4 O2 . 5_656 2.6326(18) yes Na4 O3 . 2_555 2.6422(18) yes Na4 O4 . 5_656 2.5784(19) yes Na4 O5 . 5_656 2.3374(18) yes Na4 O5 . 2_555 2.4179(18) yes Na4 O7 . 2_555 2.5575(17) yes Na4 O8 . . 2.8836(17) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 V1 O3 2_556 . 7_556 93.65(6) yes O2 V1 O6 2_556 . 2_556 89.95(6) yes O2 V1 O7 2_556 . 7_556 166.92(6) yes O2 V1 O8 2_556 . . 94.08(6) yes O2 V1 O8 2_556 . 8_555 84.85(5) yes O3 V1 O6 7_556 . 2_556 163.48(6) yes O3 V1 O7 7_556 . 7_556 86.86(6) yes O3 V1 O8 7_556 . . 96.08(6) yes O3 V1 O8 7_556 . 8_555 79.05(5) yes O6 V1 O7 2_556 . 7_556 86.05(6) yes O6 V1 O8 2_556 . . 99.74(6) yes O6 V1 O8 2_556 . 8_555 85.24(5) yes O7 V1 O8 7_556 . . 98.86(6) yes O7 V1 O8 7_556 . 8_555 82.42(5) yes O8 V1 O8 . . 8_555 174.92(6) yes O8 V1 O8 8_555 . . 174.92(6) yes O2 P1 O3 . . . 109.32(8) yes O2 P1 O4 . . . 106.86(8) yes O2 P1 O9 . . . 109.29(8) yes O3 P1 O4 . . . 109.61(8) yes O3 P1 O9 . . . 108.70(8) yes O4 P1 O9 . . . 113.00(9) yes O1 P2 O5 . . . 111.88(8) yes O1 P2 O6 . . . 107.19(8) yes O1 P2 O7 . . . 106.99(8) yes O5 P2 O6 . . . 112.14(8) yes O5 P2 O7 . . . 109.28(8) yes O6 P2 O7 . . . 109.20(8) yes O1 Na1 O2 1_655 . 2_556 116.10(6) yes O1 Na1 O3 1_655 . 2_555 114.40(6) yes O1 Na1 O5 1_655 . 5_656 94.38(6) yes O1 Na1 O8 1_655 . . 171.35(6) yes O1 Na1 O9 1_655 . 7_556 78.89(6) yes O2 Na1 O3 2_556 . 2_555 129.49(6) yes O2 Na1 O5 2_556 . 5_656 86.07(6) yes O2 Na1 O8 2_556 . . 64.56(5) yes O2 Na1 O9 2_556 . 7_556 96.35(6) yes O3 Na1 O5 2_555 . 5_656 91.08(6) yes O3 Na1 O8 2_555 . . 65.42(5) yes O3 Na1 O9 2_555 . 7_556 92.23(6) yes O5 Na1 O8 5_656 . . 94.28(6) yes O5 Na1 O9 5_656 . 7_556 173.24(7) yes O8 Na1 O9 . . 7_556 92.46(6) yes O1 Na2 O1 2_555 . 7_556 178.60(5) yes O1 Na2 O6 2_555 . 7_556 124.08(6) yes O1 Na2 O7 2_555 . 2_555 58.18(5) yes O1 Na2 O9 2_555 . . 108.16(6) yes O1 Na2 O9 2_555 . 8_554 74.76(6) yes O1 Na2 O1 7_556 . 2_555 178.60(5) yes O1 Na2 O6 7_556 . 7_556 56.30(5) yes O1 Na2 O7 7_556 . 2_555 122.72(5) yes O1 Na2 O9 7_556 . . 72.38(6) yes O1 Na2 O9 7_556 . 8_554 103.85(6) yes O6 Na2 O7 7_556 . 2_555 70.02(5) yes O6 Na2 O9 7_556 . . 116.47(6) yes O6 Na2 O9 7_556 . 8_554 115.71(6) yes O7 Na2 O9 2_555 . . 121.96(6) yes O7 Na2 O9 2_555 . 8_554 116.92(6) yes O9 Na2 O9 . . 8_554 110.45(7) yes O9 Na2 O9 8_554 . . 110.45(7) yes O1 Na3 O1 2_565 . 6_564 78.14(6) yes O1 Na3 O4 2_565 . 1_565 117.54(6) yes O1 Na3 O4 2_565 . 5_666 120.71(6) yes O1 Na3 O1 6_564 . 2_565 78.14(6) yes O1 Na3 O4 6_564 . 1_565 130.17(6) yes O1 Na3 O4 6_564 . 5_666 121.41(6) yes O4 Na3 O4 1_565 . 5_666 92.14(6) yes O4 Na3 O4 5_666 . 1_565 92.14(6) yes O2 Na4 O3 5_656 . 2_555 150.28(6) yes O2 Na4 O4 5_656 . 5_656 56.44(5) yes O2 Na4 O5 5_656 . 5_656 88.06(6) yes O2 Na4 O5 5_656 . 2_555 81.13(5) yes O2 Na4 O7 5_656 . 2_555 130.33(6) yes O2 Na4 O8 5_656 . . 150.31(6) yes O3 Na4 O4 2_555 . 5_656 152.94(6) yes O3 Na4 O5 2_555 . 5_656 85.89(6) yes O3 Na4 O5 2_555 . 2_555 88.43(6) yes O3 Na4 O7 2_555 . 2_555 63.84(5) yes O3 Na4 O8 2_555 . . 57.47(4) yes O4 Na4 O5 5_656 . 5_656 104.07(6) yes O4 Na4 O5 5_656 . 2_555 95.47(6) yes O4 Na4 O7 5_656 . 2_555 94.98(6) yes O4 Na4 O8 5_656 . . 98.08(5) yes O5 Na4 O5 5_656 . 2_555 147.26(7) yes O5 Na4 O7 5_656 . 2_555 141.10(7) yes O5 Na4 O8 5_656 . . 83.73(5) yes O5 Na4 O5 2_555 . 5_656 147.26(7) yes O5 Na4 O7 2_555 . 2_555 60.38(5) yes O5 Na4 O8 2_555 . . 119.58(6) yes O7 Na4 O8 2_555 . . 59.94(5) yes