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_1562447
_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            'Ba3 Fe2 H6 O24 P6'
_chemical_formula_weight         1099.59
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   9.4376(18)
_cell_length_b                   9.4376(18)
_cell_length_c                   36.943(7)
_cell_measurement_reflns_used    4997
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.130
_cell_measurement_theta_min      2.725
_cell_volume                     2849.6(9)
_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      295(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.971
_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  0.0254
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            4997
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.130
_diffrn_reflns_theta_min         2.725
_exptl_absorpt_coefficient_mu    8.248
_exptl_absorpt_correction_T_max  0.489
_exptl_absorpt_correction_T_min  0.367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_diffrn    3.845
_exptl_crystal_description       prism
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       0.00065(5)
_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    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         761
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+16.7218P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                752
_reflns_number_total             761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2014-212-48.cif
_cod_data_source_block           mic4
_cod_original_cell_volume        2849.6(12)
_cod_database_code               1562447
_shelx_estimated_absorpt_t_min   0.371
_shelx_estimated_absorpt_t_max   0.493
_shelxl_version_number           2013-2
_shelx_res_checksum              65737
_shelx_hkl_checksum              5635