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

data_4341265
_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            'H104 Hf11 N13 O102.5 S16'
_chemical_formula_weight         4403.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   notdet
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 102.3600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9489(5)
_cell_length_b                   30.1150(10)
_cell_length_c                   23.2134(8)
_cell_measurement_reflns_used    9696
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      32.2141
_cell_measurement_theta_min      2.2187
_cell_volume                     10208.1(6)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0425
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            178352
_diffrn_reflns_theta_full        32.24
_diffrn_reflns_theta_max         32.24
_diffrn_reflns_theta_min         1.12
_diffrn_source                   'Mo Kalpha Microfocus X-ray Source'
_diffrn_source_type              'I\mS Incoatec Mo Microfocus Source'
_exptl_absorpt_coefficient_mu    11.597
_exptl_absorpt_correction_T_max  0.35
_exptl_absorpt_correction_T_min  0.29
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    2.865
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8252
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.113
_refine_diff_density_max         8.557
_refine_diff_density_min         -5.421
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1300
_refine_ls_number_reflns         35810
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+252.1050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                29656
_reflns_number_total             35810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501841e_si_002.cif
_cod_data_source_block           Hf_11mer_Monoclinic
_cod_depositor_comments
'Adding full bibliography for 4341262--4341267.cif.'
_cod_original_formula_sum        'H104 Hf11 N13 O102.50 S16'
_cod_database_code               4341265