#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/00/2220018.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_2220018
loop_
_publ_author_name
'Schäffer, Susan J. Cline'
'Berg, Rolf W.'
_publ_section_title
;catena-Poly[tetrasodium
 [[cis-dioxido-trans-bis(sulfato-κO)molybdate(VI)]-μ-sulfato-κ²O:O']]
;
_journal_coeditor_code           WM2186
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i73
_journal_paper_doi               10.1107/S1600536808030328
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'Na4 [Mo (S O4)3 O2]'
_chemical_formula_moiety         '4(Na +), Mo O14 S3 4-'
_chemical_formula_structural     'Na4 [Mo O2 (S O4)3]'
_chemical_formula_sum            'Mo Na4 O14 S3'
_chemical_formula_weight         508.08
_chemical_name_systematic
;
catena-Poly[tetrasodium [[cis-dioxido-trans-
bis(sulfato-κO)molybdate(VI)]-μ-sulfato-κ²O:O']]
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   8.4739(6)
_cell_length_b                   9.2892(7)
_cell_length_c                   15.1046(11)
_cell_measurement_reflns_used    5457
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.57
_cell_volume                     1188.97(15)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker SMART APEX CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14125
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0.6
_diffrn_standards_interval_time  691
_diffrn_standards_number         227
_exptl_absorpt_coefficient_mu    1.855
_exptl_absorpt_correction_T_max  0.9635
_exptl_absorpt_correction_T_min  0.6650
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(SHELXTL; Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.838
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.261
_refine_ls_abs_structure_details 'Flack (1983), 1205 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0170
_refine_ls_R_factor_gt           0.0166
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0214P)²+0.3747P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0423
_reflns_number_gt                2817
_reflns_number_total             2861
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm2186.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2220018
_cod_database_fobs_code          2220018
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
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_occupancy
Mo Mo1 0.77389(2) 0.108886(19) 0.426923(11) 0.00683(5) Uani d 1
S S1 0.42167(6) 0.29669(6) 0.38157(3) 0.00770(11) Uani d 1
S S2 0.52730(7) -0.14389(6) 0.48393(3) 0.00870(11) Uani d 1
S S3 0.87553(6) 0.37753(6) 0.29746(3) 0.00819(10) Uani d 1
Na Na1 0.20072(11) 0.58268(10) 0.34042(6) 0.01293(19) Uani d 1
Na Na2 0.80653(11) 0.75841(10) 0.31656(6) 0.01239(19) Uani d 1
Na Na3 0.67303(11) 0.51270(10) 0.46834(6) 0.0144(2) Uani d 1
Na Na4 0.57005(11) 0.46216(10) 0.21305(6) 0.01274(19) Uani d 1
O O1 0.70335(19) 0.03236(17) 0.33180(10) 0.0107(3) Uani d 1
O O2 0.94651(19) 0.02131(17) 0.44263(11) 0.0119(3) Uani d 1
O O3 0.57359(18) 0.25797(17) 0.42577(11) 0.0107(3) Uani d 1
O O4 0.6456(2) -0.02040(17) 0.50576(10) 0.0116(3) Uani d 1
O O5 0.88450(19) 0.28237(18) 0.38036(10) 0.0120(3) Uani d 1
O O6 0.29354(19) 0.27689(17) 0.44854(9) 0.0096(3) Uani d 1
O O7 0.3902(2) 0.20606(18) 0.30489(10) 0.0123(3) Uani d 1
O O8 0.4313(2) 0.44896(18) 0.35609(11) 0.0124(3) Uani d 1
O O9 0.49519(19) -0.20813(17) 0.56967(11) 0.0130(3) Uani d 1
O O10 0.60611(19) -0.24259(18) 0.42327(12) 0.0147(3) Uani d 1
O O11 0.38958(19) -0.07781(18) 0.44282(11) 0.0139(3) Uani d 1
O O12 0.7888(2) 0.29908(17) 0.22934(10) 0.0124(3) Uani d 1
O O13 0.7899(2) 0.50790(17) 0.32281(10) 0.0126(3) Uani d 1
O O14 1.03833(19) 0.40786(18) 0.27218(10) 0.0133(3) Uani d 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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 -1.00 0.1200
1.00 0.00 1.00 0.1200
0.00 -1.00 1.00 0.0900
1.00 1.00 -1.00 0.0900
1.00 -1.00 -1.00 0.0100
-1.00 1.00 1.00 0.0100
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 Mo1 O1 . . 102.72(8)
O2 Mo1 O5 . . 91.81(7)
O1 Mo1 O5 . . 101.77(7)
O2 Mo1 O4 . . 95.58(7)
O1 Mo1 O4 . . 93.46(7)
O5 Mo1 O4 . . 161.18(7)
O2 Mo1 O6 . 4_556 92.71(7)
O1 Mo1 O6 . 4_556 163.68(7)
O5 Mo1 O6 . 4_556 82.77(6)
O4 Mo1 O6 . 4_556 79.62(6)
O2 Mo1 O3 . . 167.36(7)
O1 Mo1 O3 . . 89.16(7)
O5 Mo1 O3 . . 81.39(6)
O4 Mo1 O3 . . 87.91(6)
O6 Mo1 O3 4_556 . 75.92(6)
O7 S1 O8 . . 111.01(10)
O7 S1 O3 . . 111.95(9)
O8 S1 O3 . . 107.53(10)
O7 S1 O6 . . 109.52(9)
O8 S1 O6 . . 109.65(10)
O3 S1 O6 . . 107.08(9)
O9 S2 O11 . . 113.77(10)
O9 S2 O10 . . 112.83(10)
O11 S2 O10 . . 111.33(10)
O9 S2 O4 . . 103.55(9)
O11 S2 O4 . . 107.18(10)
O10 S2 O4 . . 107.52(10)
O14 S3 O12 . . 112.83(10)
O14 S3 O13 . . 112.19(10)
O12 S3 O13 . . 110.37(10)
O14 S3 O5 . . 106.14(9)
O12 S3 O5 . . 108.22(9)
O13 S3 O5 . . 106.73(10)
O12 Na1 O8 3_655 . 119.12(7)
O12 Na1 O14 3_655 1_455 115.36(7)
O8 Na1 O14 . 1_455 99.58(7)
O12 Na1 O4 3_655 4_456 131.24(7)
O8 Na1 O4 . 4_456 86.40(6)
O14 Na1 O4 1_455 4_456 98.10(6)
O12 Na1 O9 3_655 4_456 82.33(6)
O8 Na1 O9 . 4_456 141.19(7)
O14 Na1 O9 1_455 4_456 98.72(7)
O4 Na1 O9 4_456 4_456 57.26(6)
O12 Na1 O1 3_655 3_655 72.64(6)
O8 Na1 O1 . 3_655 76.04(6)
O14 Na1 O1 1_455 3_655 69.21(5)
O4 Na1 O1 4_456 3_655 155.81(6)
O9 Na1 O1 4_456 3_655 142.71(6)
O13 Na2 O14 . 3_755 130.56(7)
O13 Na2 O10 . 1_565 85.66(6)
O14 Na2 O10 3_755 1_565 143.70(7)
O13 Na2 O9 . 4_556 79.43(6)
O14 Na2 O9 3_755 4_556 98.75(7)
O10 Na2 O9 1_565 4_556 89.40(7)
O13 Na2 O7 . 3_655 78.32(6)
O14 Na2 O7 3_755 3_655 93.97(6)
O10 Na2 O7 1_565 3_655 91.17(7)
O9 Na2 O7 4_556 3_655 157.64(7)
O13 Na2 O1 . 1_565 156.46(7)
O14 Na2 O1 3_755 1_565 70.79(6)
O10 Na2 O1 1_565 1_565 73.15(6)
O9 Na2 O1 4_556 1_565 109.81(6)
O7 Na2 O1 3_655 1_565 91.70(6)
O11 Na3 O2 4_556 4_456 110.07(7)
O11 Na3 O13 4_556 . 101.80(6)
O2 Na3 O13 4_456 . 148.13(7)
O11 Na3 O10 4_556 1_565 95.79(7)
O2 Na3 O10 4_456 1_565 95.42(7)
O13 Na3 O10 . 1_565 81.85(6)
O11 Na3 O3 4_556 . 129.03(7)
O2 Na3 O3 4_456 . 75.84(6)
O13 Na3 O3 . . 83.71(6)
O10 Na3 O3 1_565 . 134.87(6)
O11 Na3 O8 4_556 . 175.92(7)
O2 Na3 O8 4_456 . 73.41(6)
O13 Na3 O8 . . 74.78(6)
O10 Na3 O8 1_565 . 81.61(6)
O3 Na3 O8 . . 53.34(5)
O7 Na4 O12 3_655 . 121.20(7)
O7 Na4 O11 3_655 3_655 90.91(6)
O12 Na4 O11 . 3_655 83.88(6)
O7 Na4 O8 3_655 . 102.80(7)
O12 Na4 O8 . . 104.28(6)
O11 Na4 O8 3_655 . 156.62(7)
O7 Na4 O1 3_655 3_655 81.21(6)
O12 Na4 O1 . 3_655 154.90(7)
O11 Na4 O1 3_655 3_655 84.66(6)
O8 Na4 O1 . 3_655 78.95(6)
O7 Na4 O13 3_655 . 78.73(6)
O12 Na4 O13 . . 58.10(6)
O11 Na4 O13 3_655 . 124.20(7)
O8 Na4 O13 . . 77.59(6)
O1 Na4 O13 3_655 . 144.70(7)
Mo1 O1 Na4 . 3_645 131.27(9)
Mo1 O1 Na2 . 1_545 110.49(7)
Na4 O1 Na2 3_645 1_545 91.78(6)
Mo1 O1 Na1 . 3_645 128.10(8)
Na4 O1 Na1 3_645 3_645 93.53(5)
Na2 O1 Na1 1_545 3_645 89.08(5)
Mo1 O2 Na3 . 4_556 147.82(9)
S1 O3 Mo1 . . 145.42(10)
S1 O3 Na3 . . 99.86(8)
Mo1 O3 Na3 . . 108.85(6)
S2 O4 Mo1 . . 131.46(9)
S2 O4 Na1 . 4_556 98.63(8)
Mo1 O4 Na1 . 4_556 127.05(8)
S3 O5 Mo1 . . 136.93(10)
S1 O6 Mo1 . 4_456 125.67(9)
S1 O7 Na4 . 3_645 129.39(10)
S1 O7 Na2 . 3_645 125.94(10)
Na4 O7 Na2 3_645 3_645 101.54(7)
S1 O8 Na1 . . 119.62(10)
S1 O8 Na4 . . 107.73(9)
Na1 O8 Na4 . . 106.56(7)
S1 O8 Na3 . . 95.05(8)
Na1 O8 Na3 . . 125.35(7)
Na4 O8 Na3 . . 100.15(7)
S2 O9 Na2 . 4_456 147.79(11)
S2 O9 Na1 . 4_556 99.36(8)
Na2 O9 Na1 4_456 4_556 99.58(7)
S2 O10 Na2 . 1_545 139.66(10)
S2 O10 Na3 . 1_545 121.13(10)
Na2 O10 Na3 1_545 1_545 91.56(6)
S2 O11 Na3 . 4_456 119.33(9)
S2 O11 Na4 . 3_645 111.58(9)
Na3 O11 Na4 4_456 3_645 128.97(8)
S3 O12 Na1 . 3_645 138.53(11)
S3 O12 Na4 . . 98.37(8)
Na1 O12 Na4 3_645 . 122.67(8)
S3 O13 Na2 . . 141.74(10)
S3 O13 Na3 . . 117.23(9)
Na2 O13 Na3 . . 92.48(6)
S3 O13 Na4 . . 93.14(8)
Na2 O13 Na4 . . 100.69(7)
Na3 O13 Na4 . . 107.34(7)
S3 O14 Na2 . 3_745 124.60(10)
S3 O14 Na1 . 1_655 124.66(10)
Na2 O14 Na1 3_745 1_655 109.32(7)
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
Mo1 O2 . 1.6905(16) y
Mo1 O1 . 1.7108(16) y
Mo1 O5 . 1.9925(16) y
Mo1 O4 . 2.0102(16) y
Mo1 O6 4_556 2.1661(15) y
Mo1 O3 . 2.1907(15) y
S1 O7 . 1.4564(16) ?
S1 O8 . 1.4681(17) ?
S1 O3 . 1.4941(16) ?
S1 O6 . 1.4953(16) ?
S2 O9 . 1.4516(17) ?
S2 O11 . 1.4575(17) ?
S2 O10 . 1.4581(17) ?
S2 O4 . 1.5589(17) ?
S3 O14 . 1.4590(17) ?
S3 O12 . 1.4595(16) ?
S3 O13 . 1.4627(16) ?
S3 O5 . 1.5346(16) ?
Na1 O12 3_655 2.2713(18) ?
Na1 O8 . 2.3273(19) ?
Na1 O14 1_455 2.3649(19) ?
Na1 O4 4_456 2.4394(18) ?
Na1 O9 4_456 2.4972(19) ?
Na1 O1 3_655 2.7652(18) ?
Na2 O13 . 2.3333(18) ?
Na2 O14 3_755 2.3350(19) ?
Na2 O10 1_565 2.3415(19) ?
Na2 O9 4_556 2.3932(19) ?
Na2 O7 3_655 2.5262(18) ?
Na2 O1 1_565 2.7006(19) ?
Na2 S3 3_755 3.3837(11) ?
Na3 O11 4_556 2.3524(19) ?
Na3 O2 4_456 2.3649(19) ?
Na3 O13 . 2.4115(18) ?
Na3 O10 1_565 2.4398(19) ?
Na3 O3 . 2.5928(19) ?
Na3 O8 . 2.724(2) ?
Na4 O7 3_655 2.3065(19) ?
Na4 O12 . 2.407(2) ?
Na4 O11 3_655 2.4078(19) ?
Na4 O8 . 2.4629(19) ?
Na4 O1 3_655 2.5003(19) ?
Na4 O13 . 2.5297(19) ?
