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_4338667
_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            'Cl8 H64 Hf4 O36'
_chemical_formula_weight         1638.07
_chemical_name_common            'hafnyl chloride octahydrate'
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   notdet
_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            2
_cell_length_a                   17.0336(12)
_cell_length_b                   17.0336(12)
_cell_length_c                   7.7023(5)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    298.(2)
_cell_measurement_theta_max      30.8498
_cell_measurement_theta_min      2.3914
_cell_volume                     2234.8(3)
_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      298.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'BRUKER APEX II CCD'
_diffrn_measurement_method       '0.5 deg w/ exposures'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            38457
_diffrn_reflns_theta_full        32.58
_diffrn_reflns_theta_max         32.58
_diffrn_reflns_theta_min         2.39
_diffrn_source                   'Mo Kalpha Microfocus X-ray Source'
_diffrn_source_type              'I\mS Incoatec Mo Microfocus Source'
_exptl_absorpt_coefficient_mu    9.830
_exptl_absorpt_correction_T_max  0.44
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    2.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.670
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.014
_refine_diff_density_min         -1.182
_refine_ls_abs_structure_details
;
Flack x determined using 1500 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.033(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         4042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0315P)^2^+2.1102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                3634
_reflns_number_total             4042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500938k_si_004.cif
_cod_data_source_block           Hf_oxychloride_octahydrate
_cod_depositor_comments
'Adding full bibliography for 4338666--4338667.cif.'
_cod_database_code               4338667