Hydrothermal synthesis and structures of the novel niobium phosphates Ba2[NbOF(PO4)2] and Ba3[Nb3O3F(PO4)4(HPO4)](H2O)7
Wang, Xiqu; Liu, Lumei; Jacobson, Allan J.; Journal of Materials Chemistry 12 (2002) 1824–; doi:10.1039/b201701f

data_7204374
_publ_section_title
;
 Hydrothermal synthesis and structures of the novel niobium phosphates
 Ba2[NbOF(PO4)2] and Ba3[Nb3O3F(PO4)4(HPO4)](H2O)7
;
_journal_issue                   6
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1824
_journal_paper_doi               10.1039/b201701f
_journal_volume                  12
_journal_year                    2002
_chemical_formula_moiety         Ba3[Nb3O3F(PO4)4(HPO4)](H2O)7
_chemical_formula_sum            'Ba3 F H14 Nb3 O30 P5'
_chemical_formula_weight         1358.71
_chemical_name_systematic
;
?
;
_space_group_IT_number           71
_symmetry_space_group_name_Hall  '-I 2 2'
_symmetry_space_group_name_H-M   'I m m m'
_atom_sites_solution_hydrogens   IGNORED
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4824(6)
_cell_length_b                   15.0067(9)
_cell_length_c                   18.4897(11)
_cell_measurement_temperature    293(2)
_cell_volume                     2631.1(3)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Siemens SMART/CCD'
_diffrn_measurement_method       'NARROW FRAME'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8275
_diffrn_reflns_theta_full        28.63
_diffrn_reflns_theta_max         28.63
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    6.115
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.6679
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2516
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.384
_refine_diff_density_min         -1.984
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       0.00044(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    IGNORED
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1786
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+42.1127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                1563
_reflns_number_total             1786
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b201701f.txt
_cod_data_source_block           Ba3[Nb3O3F(PO4)4(HPO4)](H2O)7
_cod_original_formula_sum        'H14 Ba3 F Nb3 O30 P5'
_cod_database_code               7204374