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_2100329
_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 Br1 Na9 O20 S4'
_chemical_formula_sum            'Br H4 Na9 O20 S4'
_chemical_formula_weight         739.09
_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            4
_cell_length_a                   14.9126(5)
_cell_length_b                   14.9126(5)
_cell_length_c                   8.4052(2)
_cell_measurement_reflns_used    5097
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.032
_cell_measurement_theta_min      1.018
_cell_volume                     1869.20(10)
_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    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0493
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8459
_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        32.01
_diffrn_reflns_theta_max         32.01
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    2.958
_exptl_absorpt_correction_T_max  0.8197
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.636
_refine_ls_extinction_coef       0.0047(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+1.5967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                2368
_reflns_number_total             3226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            de5022.cif
_cod_data_source_block           rgp29c
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_original_formula_sum        'Br1 H4 Na9 O20 S4'
_cod_database_code               2100329