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

data_4341264
_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            'H96 Hf11 N11 O98.5 S15'
_chemical_formula_weight         4271.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   notdet
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                88.4626(8)
_cell_angle_beta                 81.5081(8)
_cell_angle_gamma                87.5482(8)
_cell_formula_units_Z            4
_cell_length_a                   15.1165(8)
_cell_length_b                   24.5806(13)
_cell_length_c                   25.0808(13)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      32.8900
_cell_measurement_theta_min      2.7310
_cell_volume                     9206.7(8)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0353
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            155246
_diffrn_reflns_theta_full        31.51
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         2.11
_diffrn_source                   'Mo Kalpha Microfocus X-ray Source'
_diffrn_source_type              'I\mS Incoatec Mo Microfocus Source'
_exptl_absorpt_coefficient_mu    12.828
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    3.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7972
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.045
_refine_diff_density_max         9.264
_refine_diff_density_min         -3.615
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2368
_refine_ls_number_reflns         60624
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+492.3696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                51482
_reflns_number_total             60624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501841e_si_002.cif
_cod_data_source_block           Hf_11mer_Triclinic
_cod_depositor_comments
'Adding full bibliography for 4341262--4341267.cif.'
_cod_original_formula_sum        'H96 Hf11 N11 O98.50 S15'
_cod_database_code               4341264