Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_global loop_ _publ_author_name _publ_author_address '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 ; _publ_contact_author ; Dr. Andre LECLAIRE ; _publ_contact_author_address ; Laboratoire CRISMAT CNRS-UMR6508 ISMRa et Universite de Caen Bd du Marechal JUIN 14050 CAEN cedex France ; _publ_contact_author_phone '02 31 45 26 22' _publ_contact_author_fax '02 31 95 16 00' _publ_contact_author_email andre.leclaire@ismra.fr _publ_requested_journal ‘Journal of Materials Chemistry' _journal_coden_Cambridge 1145 _publ_section_title ; Hydrothermal Synthesis and Crystal Structure of a Lead Vanadium Monophosphate Hydrate with an Oprned Structure : Pb~2~V~2~O~4~(PO~4~)~2~.2H~2~O . ; data_Pb2V2O4(PO4)2-2H2O_B009367J _database_code_CSD 154003 _audit_creation_date 00-11-27 _audit_creation_method from_xtal_archive_file_using_CIFIO _chemical_compound_source 'Hydrothermal synthezis' _chemical_name_systematic ; Lead Vanadium(V) Monophosphate Hydrate ; _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_moiety 'Pb2 V2 P2 O14 H4' _chemical_formula_structural 'Pb2 V2 P2 O14 H4' _chemical_formula_sum 'Pb2 V2 P2 O14 H4' _chemical_formula_weight 806.254 _chemical_melting_point ? _computing_data_collection 'CAD-4 software' _computing_cell_refinement 'CAD-4 software' _computing_data_reduction xtal_DIFDAT_ADDREF_ABSORB _computing_structure_solution xtal _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics Atoms _computing_publication_material xtal_BONDLA_CIFIO _cell_length_a 10.0083(9) _cell_length_b 10.140(1) _cell_length_c 10.569(2) _cell_angle_alpha 90.000 _cell_angle_beta 93.89(1) _cell_angle_gamma 90.000 _cell_volume 1070.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18 _cell_measurement_theta_max 22 _cell_special_details ; ? ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_space_group_name_Hall -P_2ya loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2+x,1/2-y,z -x,-y,-z 1/2-x,1/2+y,-z _exptl_crystal_description needle _exptl_crystal_preparation Low_temperature_hydrothermal_synthesis _exptl_crystal_colour yellow _exptl_crystal_size_max 0.254 _exptl_crystal_size_mid 0.023 _exptl_crystal_size_min 0.018 _exptl_crystal_density_diffrn 4.99 _exptl_crystal_density_meas not_measured _exptl_crystal_density_method ? _exptl_crystal_F_000 1424 _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 33.45 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.3750 _exptl_absorpt_correction_T_max 0.5954 _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type xray_tube _diffrn_radiation_source 'Mo K\a' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector NaI _diffrn_measurement_device_type CAD4 _diffrn_measurement_method bisect _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% <2 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 7 2 5 6 7 0 5 6 4 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 9417 _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 44.73 _diffrn_reflns_reduction_process perpendicular_monochr_Lp loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pb ? 0 8 -4.133 10.102 ; International Tables for x-ray Crystallography (1974, Vol. IV, Table 2.3.1) ; V ? 0 8 0.267 0.530 ; 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 56 .008 .006 ; International Tables for x-ray Crystallography (1974, Vol. IV, Table 2.3.1) ; H ? 0 16 0. 0. ; International Tables for x-ray Crystallography (1974, Vol. IV, Table 2.3.1) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Pb(1) 0.42843(3) 0.60979(3) 0.15908(3) 0.01441(8) Uani d ? Pb(2) 0.45080(3) 0.02210(3) 0.70019(3) 0.01466(8) Uani d ? V(1) 0.2168(1) 0.1176(1) 0.4691(1) 0.0084(3) Uani d ? V(2) 0.2108(1) 0.4145(1) 0.9673(1) 0.0073(3) Uani d ? P(1) 0.2786(2) 0.3411(2) 0.6691(2) 0.0077(5) Uani d ? P(2) 0.4145(2) 0.1987(2) 0.0613(2) 0.0076(5) Uani d ? O(1) 0.3816(5) 0.1048(5) 0.4582(5) 0.015(2) Uani d ? O(2) 0.1991(5) 0.0417(5) 0.6051(5) 0.016(2) Uani d ? O(3) 0.1643(5) -0.0189(5) 0.3480(5) 0.014(1) Uani d ? O(4) 0.2127(5) 0.2942(5) 0.5419(5) 0.011(1) Uani d ? O(5) 0.0053(5) 0.1534(5) 0.4408(6) 0.018(2) Uani d ? O(6) 0.1971(6) 0.2446(6) 0.2957(5) 0.020(2) Uani d ? O(7) 0.3607(5) 0.4746(5) 0.9404(5) 0.011(1) Uani d ? O(8) 0.1940(5) 0.4638(5) 1.1137(5) 0.010(1) Uani d ? O(9) 0.2759(5) 0.2346(5) 0.9950(5) 0.010(1) Uani d ? O(10) 0.0997(5) 0.5555(5) 0.8891(5) 0.010(1) Uani d ? O(11) 0.0227(5) 0.3019(5) 0.9625(5) 0.010(1) Uani d ? O(13) 0.3963(5) 0.2551(5) 0.7175(5) 0.012(1) Uani d ? O(12) 0.1696(5) 0.3433(5) 0.7673(5) 0.011(1) Uani d ? O(14) 0.4507(5) 0.2891(5) 0.1715(5) 0.016(2) Uani 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 Pb(1) 0.0122(1) 0.0151(1) 0.0162(1) -0.0027(1) 0.0026(1) 0.0019(1) Pb(2) 0.0132(1) 0.0162(1) 0.0145(1) 0.0039(1) 0.0008(1) 0.0017(1) V(1) 0.0076(5) 0.0081(5) 0.0095(6) 0.0009(4) -0.0005(4) -0.0007(5) V(2) 0.0062(5) 0.0068(5) 0.0089(6) 0.0003(4) -0.0002(4) -0.0009(4) P(1) 0.0081(8) 0.0065(8) 0.0085(8) -0.0000(6) 0.0011(7) 0.0001(7) P(2) 0.0064(8) 0.0072(8) 0.0089(8) -0.0003(6) -0.0005(7) 0.0011(7) O(1) 0.009(2) 0.015(3) 0.022(3) 0.001(2) 0.004(2) 0.004(2) O(2) 0.019(3) 0.015(3) 0.014(3) -0.002(2) 0.007(2) 0.003(2) O(3) 0.014(2) 0.012(2) 0.014(3) 0.004(2) -0.004(2) -0.002(2) O(4) 0.018(3) 0.009(2) 0.006(2) -0.000(2) -0.006(2) 0.001(2) O(5) 0.008(2) 0.016(3) 0.031(3) 0.000(2) -0.001(2) -0.002(2) O(6) 0.028(3) 0.018(3) 0.013(3) -0.002(3) -0.000(2) 0.004(2) O(7) 0.008(2) 0.011(2) 0.014(2) -0.001(2) 0.003(2) -0.001(2) O(8) 0.009(2) 0.012(2) 0.011(2) -0.004(2) 0.007(2) 0.001(2) O(9) 0.003(2) 0.011(2) 0.016(3) 0.004(2) -0.004(2) 0.000(2) O(10) 0.008(2) 0.006(2) 0.015(3) 0.000(2) -0.001(2) -0.004(2) O(11) 0.005(2) 0.013(2) 0.013(3) -0.000(2) 0.003(2) -0.002(2) O(13) 0.010(2) 0.011(2) 0.015(3) 0.004(2) 0.001(2) -0.002(2) O(12) 0.008(2) 0.015(2) 0.010(2) 0.004(2) 0.005(2) -0.001(2) O(14) 0.012(3) 0.018(3) 0.018(3) 0.002(2) -0.004(2) -0.004(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 _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef .34(2) _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ; ; _refine_ls_number_reflns 2584 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0239 _refine_ls_goodness_of_fit_ref 1.341 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.0006 _refine_diff_density_min -1.78(waves_around_Pb) _refine_diff_density_max 2.22(waves_around_Pb) _geom_special_details ? 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 Pb1 O11 2.402(5) . 4_556 yes Pb1 O13 2.519(5) . 3_666 yes Pb1 O7 2.568(5) . 1_554 yes Pb1 O12 2.698(5) . 4_556 yes Pb1 O7 2.733(5) . 1_554 yes Pb1 O8 2.788(5) . 1_554 yes Pb1 O9 2.826(5) . 4_556 yes Pb1 O2 2.958(6) . 4_556 yes Pb1 O3 3.126(5) . 2 yes Pb1 O14 3.261(5) . . yes Pb2 O13 2.434(5) . . yes Pb2 O10 2.534(5) . 2 yes Pb2 O8 2.589(5) . 4_547 yes Pb2 O12 2.636(5) . 2 yes Pb2 O2 2.655(5) . . yes Pb2 O1 2.735(6) . . yes Pb2 O1 2.766(5) . 3_656 yes Pb2 O6 3.181(6) . 4_546 yes V1 O1 1.666(5) . . yes V1 O2 1.651(6) . . yes V1 O3 1.933(5) . . yes V1 O4 1.950(5) . . yes V1 O5 2.149(5) . . yes V1 O6 2.237(6) . . yes V2 O7 1.662(5) . . yes V2 O8 1.646(5) . . yes V2 O9 1.952(5) . . yes V2 O10 1.959(5) . . yes V2 O11 2.199(5) . . yes V2 O12 2.245(5) . . yes P1 O4 1.532(5) . . yes P1 O13 1.526(5) . . yes P1 O12 1.556(5) . . yes P1 O3 1.545(6) . 4_556 yes P2 O14 1.507(6) . . yes P2 O9 1.555(5) . 1_554 yes P2 O11 1.554(5) . 2_554 yes P2 O10 1.554(5) . 4_546 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 Pb1 Pb1 4.3556(7) . 3_665 no Pb1 Pb2 4.1667(6) . 3_666 no Pb1 Pb2 4.2632(5) . 4_556 no Pb1 V2 3.490(1) . 1_554 no Pb1 V2 3.608(1) . 4_556 no Pb2 V1 3.408(1) . . no 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 O2 100.9(3) . . . yes O1 V1 O3 97.2(2) . . . yes O1 V1 O4 98.4(2) . . . yes O1 V1 O5 167.0(3) . . . yes O1 V1 O6 91.2(2) . . . yes O2 V1 O3 101.6(2) . . . yes O2 V1 O4 94.5(2) . . . yes O2 V1 O5 92.1(3) . . . yes O2 V1 O6 166.6(2) . . . yes O3 V1 O4 155.0(2) . . . yes O3 V1 O5 78.9(2) . . . yes O3 V1 O6 82.2(2) . . . yes O4 V1 O5 81.5(2) . . . yes O4 V1 O6 78.0(2) . . . yes O5 V1 O6 76.0(2) . . . yes O7 V2 O8 101.5(3) . . . yes O7 V2 O9 94.2(2) . . . yes O7 V2 O10 98.8(2) . . . yes O7 V2 O11 165.4(2) . . . yes O7 V2 O12 93.9(2) . . . yes O8 V2 O9 101.4(2) . . . yes O8 V2 O10 94.8(2) . . . yes O8 V2 O11 92.2(2) . . . yes O8 V2 O12 163.5(2) . . . yes O9 V2 O10 156.8(2) . . . yes O9 V2 O11 78.2(2) . . . yes O9 V2 O12 83.1(2) . . . yes O10 V2 O11 84.8(2) . . . yes O10 V2 O12 77.0(2) . . . yes O11 V2 O12 73.1(2) . . . yes O4 P1 O13 113.1(3) . . . yes O4 P1 O12 108.0(3) . . . yes O4 P1 O3 108.9(3) . . 4_556 yes O13 P1 O12 110.2(3) . . . yes O13 P1 O3 106.4(3) . . 4_556 yes O12 P1 O3 110.3(3) . . 4_556 yes O14 P2 O9 111.5(3) . . 1_554 yes O14 P2 O11 112.3(3) . . 2_554 yes O14 P2 O10 109.3(3) . . 4_546 yes O9 P2 O11 109.8(3) 1_554 . 2_554 yes O9 P2 O10 105.8(3) 1_554 . 4_546 yes O11 P2 O10 107.9(3) 2_554 . 4_546 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min -20 _reflns_limit_l_max 20 _reflns_number_total 5828 _reflns_number_observed 2584 _reflns_observed_criterion refl_observed_if_I_>_3_sigma(I) _reflns_d_resolution_high .505 _reflns_d_resolution_low 7.301 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 9.550 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc ? ? ? ? ?