Structures of Na~9~[SO~4~]~4~<i>X</i>·2H~2~O~2~, where <i>X</i> = Cl or Br, in which the halide anions orchestrate extended orientation sequences of H~2~O~2~ solvate molecules
Pritchard, Robin Gavin; Begum, Zubeda; Lau, Yuf Fai; Austin, Jonothan; Acta Crystallographica Section B 61 (2005) 663–668; doi:10.1107/S010876810503212X

data_2100328
_publ_section_title
;
 Structures of Na~9~[SO~4~]~4~<i>X</i>&#x00B7;2H~2~O~2~, where <i>X</i>
 = Cl or Br, in which the halide anions orchestrate extended
 orientation sequences of H~2~O~2~ solvate molecules
;
_journal_coeditor_code           DE5022
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              663
_journal_page_last               668
_journal_paper_doi               10.1107/S010876810503212X
_journal_volume                  61
_journal_year                    2005
_chemical_formula_moiety         'H4 Cl1 Na9 O20 S4'
_chemical_formula_sum            'Cl H4 Na9 O20 S4'
_chemical_formula_weight         694.63
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   29.6829(3)
_cell_length_b                   29.6829(3)
_cell_length_c                   8.40180(10)
_cell_measurement_reflns_used    87529
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     7402.61(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            65291
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5504
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.534
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         8402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+19.2938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1466
_reflns_number_gt                4855
_reflns_number_total             8402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            de5022.cif
_cod_data_source_block           kc
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_original_formula_sum        'Cl1 H4 Na9 O20 S4'
_cod_database_code               2100328