#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/97/2239796.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2239796
loop_
_publ_author_name
'Weil, Matthias'
'Bonneau, Barbara'
_publ_section_title
;
 Crystal structures of Na₂SeO₄·1.5H₂O and
 Na₂SeO₄·10H₂O
;
_journal_coeditor_code           HB0010
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              54
_journal_page_last               57
_journal_paper_doi               10.1107/S1600536814011799
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'Na2 Se O4, 1.5H2 O'
_chemical_formula_structural     'Na2 Se O4, 1.5(H2 O)'
_chemical_formula_sum            'H3 Na2 O5.5 Se'
_chemical_formula_weight         215.96
_chemical_name_common            'sodium selenate sesquihydrate'
_chemical_name_systematic
;
Sodium selenate sesquihydrate
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F -2d 2'
_symmetry_space_group_name_H-M   'F 2 d d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   6.7533(8)
_cell_length_b                   8.6299(10)
_cell_length_c                   35.206(4)
_cell_measurement_reflns_used    4199
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.767
_cell_measurement_theta_min      3.875
_cell_volume                     2051.8(4)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'SMART (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'ATOMS (Dowty, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            8363
_diffrn_reflns_theta_full        32.80
_diffrn_reflns_theta_max         32.80
_diffrn_reflns_theta_min         2.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.426
_exptl_absorpt_correction_T_max  0.584
_exptl_absorpt_correction_T_min  0.488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.367
_refine_ls_abs_structure_details 'Flack (1983), 823 Friedel pairs'
_refine_ls_abs_structure_Flack   0.025(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1824
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0189
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0148P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0415
_refine_ls_wR_factor_ref         0.0420
_reflns_number_gt                1723
_reflns_number_total             1824
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb0010sup1.cf
_cod_data_source_block           1.5-hydrate
_cod_original_formula_sum        'H3 Na2 O5.50 Se'
_cod_database_code               2239796
_cod_database_fobs_code          2239796
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, -z'
'x+1/4, -y+1/4, z+1/4'
'x+1/4, y+1/4, -z+1/4'
'x, y+1/2, z+1/2'
'x, -y+1/2, -z+1/2'
'x+1/4, -y+3/4, z+3/4'
'x+1/4, y+3/4, -z+3/4'
'x+1/2, y, z+1/2'
'x+1/2, -y, -z+1/2'
'x+3/4, -y+1/4, z+3/4'
'x+3/4, y+1/4, -z+3/4'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, -z'
'x+3/4, -y+3/4, z+1/4'
'x+3/4, y+3/4, -z+1/4'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Se Se1 0.45783(6) 0.26019(2) 0.188204(5) 0.00624(5) Uani d . 1 1
Na Na1 0.94725(16) 0.40728(9) 0.15499(2) 0.01065(16) Uani d . 1 1
Na Na2 0.14581(15) 0.04335(11) 0.24656(3) 0.01009(18) Uani d . 1 1
O O1 0.6662(2) 0.35383(19) 0.19642(4) 0.0091(3) Uani d . 1 1
O O2 0.4372(3) 0.11507(17) 0.21780(4) 0.0097(3) Uani d . 1 1
O O3 0.4561(3) 0.18930(16) 0.14509(4) 0.0096(3) Uani d . 1 1
O O4 0.2752(2) 0.38446(19) 0.19358(5) 0.0095(3) Uani d . 1 1
O OW5 0.9382(3) 0.13500(18) 0.14734(4) 0.0119(3) Uani d D 1 1
O OW6 0.9204(3) 0.2500 0.2500 0.0122(5) Uani d SD 1 2
H H1 0.898(5) 0.076(3) 0.1639(7) 0.033(6) Uiso d D 1 1
H H2 1.026(4) 0.088(4) 0.1364(8) 0.033(6) Uiso d D 1 1
H H3 0.844(4) 0.232(4) 0.2676(7) 0.033(6) Uiso d D 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O2 Se1 O3 . . 107.70(7)
O2 Se1 O4 . . 111.23(9)
O3 Se1 O4 . . 110.19(9)
O2 Se1 O1 . . 109.66(8)
O3 Se1 O1 . . 110.61(9)
O4 Se1 O1 . . 107.47(8)
OW5 Na1 O3 . 4 90.74(6)
OW5 Na1 O1 . . 81.96(6)
O3 Na1 O1 4 . 86.18(7)
OW5 Na1 O3 . 13 165.30(6)
O3 Na1 O3 4 13 78.45(5)
O1 Na1 O3 . 13 106.93(7)
OW5 Na1 OW5 . 4 81.63(6)
O3 Na1 OW5 4 4 84.75(6)
O1 Na1 OW5 . 4 161.11(7)
O3 Na1 OW5 13 4 87.43(6)
OW5 Na1 O4 . 1_655 90.36(7)
O3 Na1 O4 4 1_655 164.16(7)
O1 Na1 O4 . 1_655 109.61(5)
O3 Na1 O4 13 1_655 97.35(7)
OW5 Na1 O4 4 1_655 79.79(6)
OW5 Na1 O2 . 13 135.50(6)
O3 Na1 O2 4 13 118.59(6)
O1 Na1 O2 . 13 68.66(5)
O3 Na1 O2 13 13 59.17(5)
OW5 Na1 O2 4 13 130.17(6)
O4 Na1 O2 1_655 13 70.31(5)
O2 Na2 O2 . 10_455 155.95(7)
O2 Na2 OW6 . 1_455 111.92(6)
O2 Na2 OW6 10_455 1_455 91.48(6)
O2 Na2 O4 . 6 90.30(7)
O2 Na2 O4 10_455 6 84.15(6)
OW6 Na2 O4 1_455 6 89.63(6)
O2 Na2 O1 . 13_445 79.12(6)
O2 Na2 O1 10_455 13_445 91.76(6)
OW6 Na2 O1 1_455 13_445 126.16(6)
O4 Na2 O1 6 13_445 144.12(7)
Se1 O1 Na2 . 13 114.37(8)
Se1 O1 Na1 . . 130.73(9)
Na2 O1 Na1 13 . 110.74(7)
Se1 O2 Na2 . . 124.06(9)
Se1 O2 Na2 . 10 137.82(10)
Na2 O2 Na2 . 10 97.03(5)
Se1 O2 Na1 . 13_445 89.17(6)
Na2 O2 Na1 . 13_445 101.13(6)
Na2 O2 Na1 10 13_445 91.96(6)
Se1 O3 Na1 . 16_445 135.64(11)
Se1 O3 Na1 . 13_445 103.80(7)
Na1 O3 Na1 16_445 13_445 90.39(6)
Se1 O4 Na2 . 6 123.44(9)
Se1 O4 Na1 . 1_455 128.80(9)
Na2 O4 Na1 6 1_455 97.50(6)
Na1 OW5 Na1 . 16_445 91.42(7)
Na1 OW5 H1 . . 123(2)
Na1 OW5 H1 16_445 . 111(2)
Na1 OW5 H2 . . 122(3)
Na1 OW5 H2 16_445 . 100(2)
H1 OW5 H2 . . 106(3)
Na2 OW6 Na2 6_655 1_655 99.15(10)
Na2 OW6 H3 6_655 . 121(3)
Na2 OW6 H3 1_655 . 108(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Na1 OW5 . 2.3660(18) y
Na1 O3 4 2.4157(19) y
Na1 O1 . 2.4379(18) y
Na1 O3 13 2.4594(16) y
Na1 OW5 4 2.465(2) y
Na1 O4 1_655 2.6057(19) y
Na1 O2 13 2.8475(17) y
Na2 O2 . 2.298(2) y
Na2 O2 10_455 2.3301(18) y
Na2 OW6 1_455 2.3480(18) y
Na2 O4 6 2.3651(19) y
Na2 O1 13_445 2.4103(18) y
Se1 O2 . 1.6350(14) y
Se1 O3 . 1.6367(14) y
Se1 O4 . 1.6451(16) y
Se1 O1 . 1.6481(15) y
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
OW5 H1 O4 13_545 0.8199(10) 2.125(9) 2.922(2) 164(3)
OW5 H2 O3 16_545 0.8200(10) 2.082(7) 2.891(2) 169(3)
OW6 H3 O1 6 0.8201(10) 1.898(8) 2.703(2) 167(4)
