Synthesis and characterization of novel barium iron phosphates: Insight into new structure types tailored by hydrogen atoms
Sun, Li-Zhi; Sun, Wei; Ren, Wei-Jian; Zhang, Jia-Ying; Huang, Ya-Xi; Sun, Zhi-Mei; Pan, Yuanming; Mi, Jin-Xiao; Journal of Solid State Chemistry 212 (2014) 48–57; doi:10.1016/j.jssc.2014.01.010

data_1562444
_publ_section_title
;
 Synthesis and characterization of novel barium iron phosphates: Insight
 into new structure types tailored by hydrogen atoms
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              48
_journal_page_last               57
_journal_paper_doi               10.1016/j.jssc.2014.01.010
_journal_volume                  212
_journal_year                    2014
_chemical_formula_sum            'Ba Fe H2 O11 P3'
_chemical_formula_weight         464.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                101.237(4)
_cell_angle_beta                 96.874(3)
_cell_angle_gamma                106.472(4)
_cell_formula_units_Z            2
_cell_length_a                   7.6547(13)
_cell_length_b                   8.6601(15)
_cell_length_c                   6.8717(12)
_cell_measurement_reflns_used    3510
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.203
_cell_measurement_theta_min      2.527
_cell_volume                     420.98(13)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
'DIAMOND (Brandenburg, 2011) & ATOMS (Dowty, 2004)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type
'Bruker SMART APEX CCD area-detector diffractometer'
_diffrn_measurement_method
'1800 images,\f = 0, 90, 180\%, \c = 54.74\%, \D\w=0.3\%, Exp time: 15 s.'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3510
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        26.500
_diffrn_reflns_theta_max         28.203
_diffrn_reflns_theta_min         2.527
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.997
_exptl_absorpt_correction_T_max  0.335
_exptl_absorpt_correction_T_min  0.193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_diffrn    3.661
_exptl_crystal_description       prism
_exptl_crystal_F_000             434
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.230
_refine_diff_density_min         -1.486
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       0.0450(19)
_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   1.000
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         1862
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.7771P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0714
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1846
_reflns_number_total             1862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2014-212-48.cif
_cod_data_source_block           micn
_cod_database_code               1562444
_shelx_estimated_absorpt_t_min   0.193
_shelx_estimated_absorpt_t_max   0.335
_shelxl_version_number           2013-2
_shelx_res_checksum              86756
_shelx_hkl_checksum              83754