# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 1145/269 data_kwp2o8_B007592M _publ_contact_author #ActaC ; Dr. Andr\e LECLAIRE ; _publ_contact_author_address ; Laboratoire CRISMAT CNRS-UMR6508 ISMRa et Universit\e de Caen Bd du Mar\echal JUIN 14050 CAEN cedex France ; _publ_contact_author_phone '02 31 45 26 22' #ActaC _publ_contact_author_fax '02 31 95 16 00' #ActaC _publ_contact_author_email andre.leclaire@ismra.fr #ActaC _publ_requested_journal 'Journal of Materials Chemistry' #ActaC _publ_section_title #ActaC ; Stabilization of the tungstyl ion configuration : the W(V) diphosphate KWOP~2~O~7~. ; _audit_creation_date 00-10-02 _audit_creation_method from_xtal_archive_file_using_CIFIO _chemical_compound_source 'Solid state synthezis' #ActaC _chemical_name_systematic #ActaC ; Potassium tungsten(V) diphosphate ; _chemical_name_common ? #ActaC _chemical_formula_analytical ? #ActaC _chemical_formula_moiety 'K W P2 O8' #ActaC _chemical_formula_structural 'K W O P2 O7' #ActaC _chemical_formula_sum 'K W P2 O8' #ActaC _chemical_formula_weight 412.89 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'CAD-4 software' #ActaC _computing_cell_refinement 'CAD-4 software' #ActaC _computing_data_reduction xtal_DIFDAT_ADDREF_ABSORB #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics Atoms #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 5.0629(3) #ActaC _cell_length_b 11.770(2) #ActaC _cell_length_c 11.551(1) #ActaC _cell_angle_alpha 90.000 #ActaC _cell_angle_beta 91.039(6) #ActaC _cell_angle_gamma 90.000 #ActaC _cell_volume 688.2(1) #ActaC _cell_formula_units_Z 4 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 25 #ActaC _cell_measurement_theta_min 18 #ActaC _cell_measurement_theta_max 22 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting orthorhombic #ActaC _symmetry_space_group_name_H-M 'P 1 21/n 1' #ActaC _symmetry_space_group_name_Hall -P_2yn #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _exptl_crystal_description needle #ActaC _exptl_crystal_preparation solid_state_reaction _exptl_crystal_colour green #ActaC _exptl_crystal_size_max 0.195 #ActaC _exptl_crystal_size_mid 0.027 #ActaC _exptl_crystal_size_min 0.018 #ActaC _exptl_crystal_density_diffrn 3.895 #ActaC _exptl_crystal_density_meas not_measured #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 748.00 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 17.86 #ActaC _exptl_absorpt_correction_type gaussian #ActaC _exptl_absorpt_correction_T_min 0.5468 #ActaC _exptl_absorpt_correction_T_max 0.7150 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type xray_tube #ActaC _diffrn_radiation_source 'Mo K\a' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector NaI #ActaC _diffrn_measurement_device_type CAD4 #ActaC _diffrn_measurement_method bisect #ActaC _diffrn_standards_number 3 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 60 #ActaC _diffrn_standards_decay_% <2 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC 3 8 1 4 0 6 2 6 7 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 6023 #ActaC _diffrn_reflns_av_R_equivalents 0 #ActaC _diffrn_reflns_av_sigmaI/netI ? #ActaC _diffrn_reflns_limit_h_min -10 #ActaC _diffrn_reflns_limit_h_max 10 #ActaC _diffrn_reflns_limit_k_min 0 #ActaC _diffrn_reflns_limit_k_max 23 #ActaC _diffrn_reflns_limit_l_min 0 #ActaC _diffrn_reflns_limit_l_max 22 #ActaC _diffrn_reflns_theta_min 3.46 #ActaC _diffrn_reflns_theta_max 44.91 #ActaC _diffrn_reflns_reduction_process perpendicular_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC K ? 0 4 .179 .25 ; International Tables for x-ray Crystallography (1974, Vol. IV, Table 2.3.1) ; W ? 0 4 -1.421 6.872 ; International Tables for x-ray Crystallography (1974, Vol. IV, Table 2.3.1) ; P ? 0 8 .09 .095 ; International Tables for x-ray Crystallography (1974, Vol. IV, Table 2.3.1) ; O ? 0 32 .008 .006 ; International Tables for x-ray Crystallography (1974, Vol. IV, Table 2.3.1) ; loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC W1 0.26183(5) 0.11761(2) 0.16749(2) 0.00593(5) Uani d ? P1 0.7520(4) 0.4345(2) 0.3671(2) 0.0067(4) Uani d ? P2 0.7664(4) 0.3054(2) 0.1511(2) 0.0070(4) Uani d ? K1 0.7734(4) 0.1295(2) 0.4494(2) 0.239(5) Uani d ? O1 0.312(1) 0.1291(6) 0.3118(5) 0.020(2) Uani d ? O2 0.052(1) 0.2616(5) 0.1455(5) 0.014(1) Uani d ? O3 0.573(1) 0.2112(5) 0.1179(5) 0.012(1) Uani d ? O4 -0.071(1) 0.0248(5) 0.1817(4) 0.011(1) Uani d ? O5 0.460(1) -0.0284(5) 0.1434(5) 0.014(1) Uani d ? O6 0.187(1) 0.1080(5) -0.0144(4) 0.014(1) Uani d ? O7 0.719(1) 0.3234(4) 0.2883(5) 0.011(1) Uani d ? O8 0.730(1) 0.4116(5) 0.0863(5) 0.017(2) Uani d ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC W1 .00244(8) .00772(9) .00762(9) -.0007(1) .00013(5) -.0016(1) P1 .0049(7) .0071(7) .0080(7) .0007(6) .0004(6) -.0005(6) P2 .0045(7) .0061(7) .0103(9) -.0002(6) .0010(6) -.0020(6) K1 .0250(9) .0173(9) .0289(9) .0018(7) -.0096(7) -.0031(8) O1 .016(2) .031(4) .013(2) -.002(3) -.001(2) .004(3) O2 .003(2) .012(2) .027(3) .002(2) .001(2) -.001(2) O3 .005(2) .014(2) .017(2) -.005(2) .003(2) -.003(2) O4 .006(2) .013(2) .013(2) -.004(2) -.001(2) .000(2) O5 .008(2) .010(2) .025(3) .001(2) -.000(2) .001(2) O6 .012(2) .019(3) .010(2) -.000(2) .001(2) .001(2) O7 .013(2) .006(2) .015(2) -.002(2) .003(2) -.000(2) O8 .020(3) .010(2) .022(3) .001(2) .002(2) .005(2) _atom_sites_solution_primary 'Heavy atom method ' _atom_sites_solution_secondary 'Fourier differences' _atom_sites_solution_hydrogens ? _refine_special_details ? _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment ? #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef .31(3) #ActaC _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ; Refinement of the two enanthiomorphic solutions ; _refine_ls_number_reflns 2648 #ActaC _refine_ls_number_parameters 110 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_gt 0.0357 #ActaC _refine_ls_wR_factor_ref 0.0356 #ActaC _refine_ls_goodness_of_fit_ref 1.811 #ActaC _refine_ls_shift/su_max 0.001 #ActaC _refine_ls_shift/su_mean 0.00007 #ActaC _refine_diff_density_min -6.29(waves_around_W) #ActaC _refine_diff_density_max 6.05(waves_around_W) #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC W1 O1 1.687(5) . . yes W1 O2 2.013(5) . . yes W1 O3 2.013(6) . . yes W1 O4 2.019(5) . . yes W1 O5 2.012(5) . . yes W1 O6 2.131(5) . . yes P1 O4 1.506(6) . 2 yes P1 O5 1.528(5) . 2_655 yes P1 O6 1.499(5) . . yes P1 O7 1.601(5) . 4 yes P2 O3 1.523(6) . . yes P2 O2 1.538(5) . 1_655 yes P2 O7 1.622(6) . . yes P2 O8 1.467(6) . . yes K1 O8 2.598(6) . 2_645 yes K1 O1 2.802(6) . . yes K1 O8 2.8186) . 4 yes K1 O2 2.850(6) . 4 yes K1 O7 2.954(6) . . yes K1 O3 3.082(6) . 4 yes K1 O6 3.150(7) . 4 yes K1 O1 3.180(6) . 1_655 yes K1 O8 3.236(6) . 4_455 yes loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC P1 P2 2.924(3) . . yes K1 K1 3.978(3) . 3_756 yes O1 O2 2.786(8) . . no O1 O3 2.793(8) . . no O1 O4 2.724(8) . . no O1 O5 2.779(8) . . no O2 O3 2.726(7) . . no O2 O4 2.889(8) . . no O2 O6 2.682(8) . . no O2 O3 2.513(7) . 1_455 no O2 O7 2.490(8) . 1_455 no O2 O8 2.492(8) . 1_455 no O3 O5 2.892(8) . . no O3 O6 2.744(7) . . no O3 O4 2.925(7) . 1_655 no O3 O7 2.471(7) . . no O3 O8 2.517(8) . . no O4 O5 2.806(7) . . no O4 O6 2.811(7) . . no O4 O5 2.485(7) . 1_455 no O4 O6 2.545(8) . 3 no O4 O7 2.511(7) . 2_545 no O5 O6 2.779(8) . . no O5 O6 2.528(8) . 3_655 no O5 O7 2.503(7) . 2_645 no O6 O7 2.427(7) . 4_454 no O7 O8 2.555(8) . . no loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC O1 W1 O2 97.3(3) . . . yes O1 W1 O3 97.6(3) . . . yes O1 W1 O4 94.2(3) . . . yes O1 W1 O5 98.0(3) . . . yes O1 W1 O6 177.8(3) . . . yes O2 W1 O3 85.2(2) . . . yes O2 W1 O4 91.5(2) . . . yes O2 W1 O5 164.7(2) . . . yes O2 W1 O6 80.6(2) . . . yes O3 W1 O4 168.0(2) . . . yes O3 W1 O5 91.9(2) . . . yes O3 W1 O6 82.8(2) . . . yes O4 W1 O5 88.2(2) . . . yes O4 W1 O6 85.2(2) . . . yes O5 W1 O6 84.2(2) . . . yes O4 P1 O5 110.0(3) 2 . 2_655 yes O4 P1 O6 115.8(3) 2 . 4 yes O4 P1 O7 107.8(3) 2 . . yes O5 P1 O6 113.2(3) 2_655 . 4 yes O5 P1 O7 106.2(3) 2_655 . . yes O6 P1 O7 103.0(3) 4 . . yes O2 P2 O3 110.3(3) 1_655 . . yes O2 P2 O7 104.0(3) 1_655 . . yes O2 P2 O8 112.0(3) 1_655 . . yes O3 P2 O7 103.5(3) . . . yes O3 P2 O8 114.6(3) . . . yes O7 P2 O8 111.5(3) . . . yes P1 O7 P2 130.3(3) . . . yes loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _reflns_number_total 5828 #ActaC _reflns_number_observed 2648 #ActaC _reflns_observed_criterion refl_observed_if_I_>_3_sigma(I) _reflns_d_resolution_high .506 _reflns_d_resolution_low 5.888 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 6.621 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc ? ? ? ? ? loop_ _publ_author_name #ActaC _publ_author_address #ActaC 'Leclaire, A.' ; Laboratoire CRISMAT CNRS-UMR6508 ISMRa et Universit\e de Caen Bd du Mar\echal JUIN 14050 CAEN cedex France ; 'Chardon, J.' ; Laboratoire CRISMAT CNRS-UMR6508 ISMRa et Universit\e de Caen Bd du Mar\echal JUIN 14050 CAEN cedex France ; 'Raveau, B.' ; Laboratoire CRISMAT CNRS-UMR6508 ISMRa et Universit\e de Caen Bd du Mar\echal JUIN 14050 CAEN cedex France ;