Aqueous hafnium sulfate chemistry: structures of crystalline precipitates.
Kalaji, Ali; Soderholm, L.; Inorganic chemistry 53 (2014) 11252–11260; doi:10.1021/ic501841e

data_4341267
_publ_section_title
;
 Aqueous hafnium sulfate chemistry: structures of crystalline
 precipitates.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11252
_journal_page_last               11260
_journal_paper_doi               10.1021/ic501841e
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'H49 Hf6 N7 O57.5 S10.5'
_chemical_formula_weight         2475.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_Hall           '-P 2ab 2a'
_space_group_name_H-M_alt        'P m m n'
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_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                   19.0716(7)
_cell_length_b                   9.9058(4)
_cell_length_c                   14.1053(5)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      32.9754
_cell_measurement_theta_min      2.3168
_cell_volume                     2664.77(17)
_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 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0286
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46419
_diffrn_reflns_theta_full        33.18
_diffrn_reflns_theta_max         33.18
_diffrn_reflns_theta_min         1.44
_diffrn_source                   'Mo Kalpha Microfocus X-ray Source'
_diffrn_source_type              'I\mS Incoatec Mo Microfocus Source'
_exptl_absorpt_coefficient_mu    12.190
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    3.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.037
_refine_diff_density_max         2.839
_refine_diff_density_min         -2.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5289
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0223
_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^)+(0.0253P)^2^+10.1969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0557
_reflns_number_gt                4873
_reflns_number_total             5289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501841e_si_002.cif
_cod_data_source_block           Hf_Hexamer_Small
_cod_depositor_comments
'Adding full bibliography for 4341262--4341267.cif.'
_cod_original_formula_sum        'H49 Hf6 N7 O57.50 S10.50'
_cod_database_code               4341267