Changing Hafnium Speciation in Aqueous Sulfate Solutions: A High-Energy X-ray Scattering Study.
Kalaji, Ali; Skanthakumar, S.; Kanatzidis, Mercouri G.; Mitchell, John F.; Soderholm, L.; Inorganic chemistry 53 (2014) 6321–6328; doi:10.1021/ic500938k

data_4338666
_publ_section_title
;
 Changing Hafnium Speciation in Aqueous Sulfate Solutions: A High-Energy
 X-ray Scattering Study.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6321
_journal_page_last               6328
_journal_paper_doi               10.1021/ic500938k
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'H8 Hf O12 S2'
_chemical_formula_weight         442.67
_chemical_name_common            'Hafnium sulfate tetrahydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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                90
_cell_formula_units_Z            8
_cell_length_a                   5.48840(10)
_cell_length_b                   11.6086(3)
_cell_length_c                   25.8710(7)
_cell_measurement_reflns_used    5805
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      33.0271
_cell_measurement_theta_min      3.1496
_cell_volume                     1648.31(7)
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'XS, SHELXTL Ver. 6.12 (Bruker 2001)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'BRUKER APEX II CCD'
_diffrn_measurement_method       '0.3 deg w/ exposures'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            6639
_diffrn_reflns_theta_full        32.56
_diffrn_reflns_theta_max         32.56
_diffrn_reflns_theta_min         3.15
_diffrn_source                   'Mo Kalpha Microfocus X-ray Source'
_diffrn_source_type              'I\mS Incoatec Mo Microfocus Source'
_exptl_absorpt_coefficient_mu    13.230
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    3.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.404
_refine_diff_density_min         -1.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.328
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.328
_refine_ls_R_factor_all          0.0110
_refine_ls_R_factor_gt           0.0108
_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^)+(0.0117P)^2^+5.6329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0259
_refine_ls_wR_factor_ref         0.0259
_reflns_number_gt                747
_reflns_number_total             753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500938k_si_005.cif
_cod_data_source_block           Hf_sulfate_tetrahydrate
_cod_depositor_comments
'Adding full bibliography for 4338666--4338667.cif.'
_cod_database_code               4338666