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

data_4341266
_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            'H43 Hf6 N7 O54.5 S10.5'
_chemical_formula_weight         2420.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   22.5768(6)
_cell_length_b                   9.8962(3)
_cell_length_c                   23.7620(6)
_cell_measurement_reflns_used    9746
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      33.0435
_cell_measurement_theta_min      2.4050
_cell_volume                     5309.0(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      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0291
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            92221
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         1.24
_diffrn_source                   'Mo Kalpha Microfocus X-ray Source'
_diffrn_source_type              'I\mS Incoatec Mo Microfocus Source'
_exptl_absorpt_coefficient_mu    12.230
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    3.029
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4512
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.040
_refine_diff_density_max         5.616
_refine_diff_density_min         -3.807
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.261
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         10329
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.269
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+150.0456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1025
_reflns_number_gt                9891
_reflns_number_total             10329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501841e_si_002.cif
_cod_data_source_block           Hf_Hexamer_Large
_cod_depositor_comments
'Adding full bibliography for 4341262--4341267.cif.'
_cod_original_formula_sum        'H43 Hf6 N7 O54.50 S10.50'
_cod_database_code               4341266