In Situ Characterization of Elusive Salt Hydrates-The Crystal Structures of the Heptahydrate and Octahydrate of Sodium Sulfate
Iain D. H. Oswald; Andrea Hamilton; Christopher Hall; William G. Marshall; Timothy J. Prior; Colin R. Pulham; Journal of the American Chemical Society 130 (2008) 17795–17800; doi:10.1021/ja805429m

data_4108920
_publ_section_title
;
 In Situ Characterization of Elusive Salt Hydrates-The Crystal Structures
 of the Heptahydrate and Octahydrate of Sodium Sulfate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17795
_journal_page_last               17800
_journal_paper_doi               10.1021/ja805429m
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'Na2 S1 O4 7(H2O) '
_chemical_formula_sum            'H14 Na2 O11 S'
_chemical_formula_weight         266.13
_space_group_IT_number           141
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_space_group_name_H-M   'I 41/a m d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-04-30
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1413(2)
_cell_length_b                   7.1413(2)
_cell_length_c                   22.1101(11)
_cell_measurement_reflns_used    6856
_cell_measurement_temperature    150
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1127.57(7)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            6163
_diffrn_reflns_theta_full        28.789
_diffrn_reflns_theta_max         29.679
_diffrn_reflns_theta_min         2.998
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.48
_refine_ls_extinction_coef       96(17)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         453
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.001730
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.00P)^2^ + 3.99P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1190
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1190
_reflns_limit_h_max              7
_reflns_limit_h_min              0
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                426
_reflns_number_total             453
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.07
_oxford_diffrn_Wilson_scale      6.15
_oxford_refine_ls_r_factor_ref   0.0432
_oxford_refine_ls_scale          0.519(4)
_oxford_reflns_number_all        453
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'cp7019 in I4(1)/amd'
_cod_data_source_file            ja805429m_si_001.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'I 41/a m d '
_cod_original_formula_sum        'H14 Na2 O11 S1'
_cod_database_code               4108920