#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/43/7204321.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7204321
loop_
_publ_author_name
'Yeates, Rachel M.'
'Harrison, William T. A.'
_publ_section_title
;
 Synthesis, crystal structure and properties of
 Na3Zn4O(AsO4)3·6H2O, a new framework zincoarsenate
;
_journal_issue                   4
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1103
_journal_paper_doi               10.1039/b110288e
_journal_volume                  12
_journal_year                    2002
_chemical_formula_sum            'As3 H12 Na3 O19 Zn4'
_chemical_formula_weight         871.31
_chemical_melting_point          'decomposes before melting'
_chemical_name_common            'Sodium zinc arsenate'
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   10.9493(5)
_cell_length_b                   10.9493(5)
_cell_length_c                   26.7099(13)
_cell_measurement_reflns_used    3933
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      32.20
_cell_measurement_theta_min      2.64
_cell_volume                     2773.2(2)
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SMART (Bruker, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART1000'
_diffrn_measurement_method       ω
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            7427
_diffrn_reflns_theta_full        32.51
_diffrn_reflns_theta_max         32.51
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    10.617
_exptl_absorpt_correction_T_max  0.3390
_exptl_absorpt_correction_T_min  0.3390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.023(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         2095
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0166P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0423
_reflns_number_gt                1954
_reflns_number_total             2095
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b110288e.txt
_cod_data_source_block           nza2
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_original_formula_sum        'H12 As3 Na3 O19 Zn4'
_cod_database_code               7204321
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.39571(18) 0.50320(19) 0.05957(6) 0.0432(4) Uani 1 1 d . . .
Zn1 Zn 0.0000 0.0000 0.00001(2) 0.01237(11) Uani 1 3 d S . .
Zn2 Zn 0.19725(3) 0.10832(3) 0.095521(11) 0.01206(7) Uani 1 1 d . . .
As1 As 0.32341(3) 0.18135(3) -0.016944(11) 0.01278(6) Uani 1 1 d . . .
O1 O 0.0000 0.0000 0.07307(13) 0.0130(6) Uani 1 3 d S . .
O2 O 0.2377(2) 0.3004(2) 0.10714(8) 0.0192(4) Uani 1 1 d . . .
O3 O 0.2392(2) 0.0198(2) 0.15156(8) 0.0213(4) Uani 1 1 d . . .
O4 O 0.3146(2) 0.1093(3) 0.03986(8) 0.0194(4) Uani 1 1 d . . .
O5 O 0.1650(2) 0.1593(2) -0.03174(8) 0.0199(4) Uani 1 1 d . . .
O6 O 0.5784(3) 0.4417(3) 0.08165(13) 0.0448(8) Uani 1 1 d . . .
H61 H 0.6293 0.5344 0.0739 0.054 Uiso 1 1 d R . .
H62 H 0.6062 0.3927 0.0645 0.054 Uiso 1 1 d R . .
O7 O 0.5344(3) 0.7197(3) 0.01635(10) 0.0343(6) Uani 1 1 d . . .
H71 H 0.5241 0.7251 -0.0181 0.041 Uiso 1 1 d R . .
H72 H 0.6173 0.7075 0.0223 0.041 Uiso 1 1 d R . .
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Na1 O2 171.91(12) . . ?
O7 Na1 O7 90.98(15) . 3_565 ?
O2 Na1 O7 84.83(10) . 3_565 ?
O7 Na1 O6 100.74(12) . . ?
O2 Na1 O6 85.93(10) . . ?
O7 Na1 O6 153.57(12) 3_565 . ?
O7 Na1 O5 80.30(10) . 18_554 ?
O2 Na1 O5 96.04(9) . 18_554 ?
O7 Na1 O5 121.98(11) 3_565 18_554 ?
O6 Na1 O5 83.59(10) . 18_554 ?
O7 Na1 O3 91.35(10) . 11_554 ?
O2 Na1 O3 95.62(9) . 11_554 ?
O7 Na1 O3 90.82(10) 3_565 11_554 ?
O6 Na1 O3 65.52(10) . 11_554 ?
O5 Na1 O3 145.99(9) 18_554 11_554 ?
O7 Na1 As1 144.22(10) . 16_554 ?
O2 Na1 As1 27.99(5) . 16_554 ?
O7 Na1 As1 79.23(8) 3_565 16_554 ?
O6 Na1 As1 103.07(9) . 16_554 ?
O5 Na1 As1 76.27(6) 18_554 16_554 ?
O3 Na1 As1 122.80(7) 11_554 16_554 ?
O7 Na1 Zn1 94.31(8) . 16_554 ?
O2 Na1 Zn1 79.09(6) . 16_554 ?
O7 Na1 Zn1 93.57(8) 3_565 16_554 ?
O6 Na1 Zn1 108.90(9) . 16_554 ?
O5 Na1 Zn1 31.80(5) 18_554 16_554 ?
O3 Na1 Zn1 172.77(7) 11_554 16_554 ?
As1 Na1 Zn1 52.72(3) 16_554 16_554 ?
O7 Na1 Na1 37.42(8) . 2_665 ?
O2 Na1 Na1 134.97(7) . 2_665 ?
O7 Na1 Na1 84.85(8) 3_565 2_665 ?
O6 Na1 Na1 118.59(10) . 2_665 ?
O5 Na1 Na1 54.68(6) 18_554 2_665 ?
O3 Na1 Na1 128.23(6) 11_554 2_665 ?
As1 Na1 Na1 106.98(4) 16_554 2_665 ?
Zn1 Na1 Na1 58.01(2) 16_554 2_665 ?
O7 Na1 Na1 85.39(8) . 3_565 ?
O2 Na1 Na1 87.13(9) . 3_565 ?
O7 Na1 Na1 36.66(8) 3_565 3_565 ?
O6 Na1 Na1 166.23(9) . 3_565 ?
O5 Na1 Na1 85.33(6) 18_554 3_565 ?
O3 Na1 Na1 127.10(7) 11_554 3_565 ?
As1 Na1 Na1 66.22(4) 16_554 3_565 ?
Zn1 Na1 Na1 58.01(2) 16_554 3_565 ?
Na1 Na1 Na1 60.0 2_665 3_565 ?
O7 Na1 H61 80.5 . . ?
O2 Na1 H61 105.6 . . ?
O7 Na1 H61 160.4 3_565 . ?
O6 Na1 H61 21.2 . . ?
O5 Na1 H61 74.1 18_554 . ?
O3 Na1 H61 72.0 11_554 . ?
As1 Na1 H61 117.7 16_554 . ?
Zn1 Na1 H61 104.5 16_554 . ?
Na1 Na1 H61 98.3 2_665 . ?
Na1 Na1 H61 156.7 3_565 . ?
O7 Na1 H72 23.0 . . ?
O2 Na1 H72 163.1 . . ?
O7 Na1 H72 111.8 3_565 . ?
O6 Na1 H72 77.7 . . ?
O5 Na1 H72 78.0 18_554 . ?
O3 Na1 H72 81.6 11_554 . ?
As1 Na1 H72 154.0 16_554 . ?
Zn1 Na1 H72 102.0 16_554 . ?
Na1 Na1 H72 53.3 2_665 . ?
Na1 Na1 H72 107.9 3_565 . ?
H61 Na1 H72 57.6 . . ?
O1 Zn1 O5 115.53(7) . 2 ?
O1 Zn1 O5 115.53(7) . 3 ?
O5 Zn1 O5 102.79(8) 2 3 ?
O1 Zn1 O5 115.53(7) . . ?
O5 Zn1 O5 102.79(8) 2 . ?
O5 Zn1 O5 102.79(8) 3 . ?
O1 Zn1 Na1 142.29(3) . 10_554 ?
O5 Zn1 Na1 101.25(7) 2 10_554 ?
O5 Zn1 Na1 43.71(7) 3 10_554 ?
O5 Zn1 Na1 60.33(7) . 10_554 ?
O1 Zn1 Na1 142.29(3) . 11_444 ?
O5 Zn1 Na1 43.71(7) 2 11_444 ?
O5 Zn1 Na1 60.33(7) 3 11_444 ?
O5 Zn1 Na1 101.25(7) . 11_444 ?
Na1 Zn1 Na1 63.97(4) 10_554 11_444 ?
O1 Zn1 Na1 142.29(3) . 12_454 ?
O5 Zn1 Na1 60.33(7) 2 12_454 ?
O5 Zn1 Na1 101.25(7) 3 12_454 ?
O5 Zn1 Na1 43.71(7) . 12_454 ?
Na1 Zn1 Na1 63.97(4) 10_554 12_454 ?
Na1 Zn1 Na1 63.97(4) 11_444 12_454 ?
O2 Zn2 O3 115.50(9) . . ?
O2 Zn2 O4 108.71(10) . . ?
O3 Zn2 O4 105.47(9) . . ?
O2 Zn2 O1 106.74(7) . . ?
O3 Zn2 O1 113.13(9) . . ?
O4 Zn2 O1 106.91(11) . . ?
O5 As1 O3 111.46(11) . 11_554 ?
O5 As1 O2 108.51(10) . 10_554 ?
O3 As1 O2 110.45(11) 11_554 10_554 ?
O5 As1 O4 109.34(11) . . ?
O3 As1 O4 108.77(12) 11_554 . ?
O2 As1 O4 108.25(12) 10_554 . ?
O5 As1 Na1 68.03(8) . 10_554 ?
O3 As1 Na1 135.81(8) 11_554 10_554 ?
O2 As1 Na1 41.73(7) 10_554 10_554 ?
O4 As1 Na1 112.75(9) . 10_554 ?
Zn1 O1 Zn2 107.75(9) . . ?
Zn1 O1 Zn2 107.75(9) . 3 ?
Zn2 O1 Zn2 111.14(9) . 3 ?
Zn1 O1 Zn2 107.75(9) . 2 ?
Zn2 O1 Zn2 111.14(9) . 2 ?
Zn2 O1 Zn2 111.14(9) 3 2 ?
As1 O2 Zn2 123.49(12) 16_554 . ?
As1 O2 Na1 110.28(11) 16_554 . ?
Zn2 O2 Na1 126.00(11) . . ?
As1 O3 Zn2 120.81(12) 17_544 . ?
As1 O3 Na1 112.87(10) 17_544 17_544 ?
Zn2 O3 Na1 124.18(10) . 17_544 ?
As1 O4 Zn2 124.56(13) . . ?
As1 O5 Zn1 116.82(11) . . ?
As1 O5 Na1 135.15(11) . 12_454 ?
Zn1 O5 Na1 104.49(9) . 12_454 ?
Na1 O6 H61 76.7 . . ?
Na1 O6 H62 128.5 . . ?
H61 O6 H62 111.4 . . ?
Na1 O7 Na1 105.91(13) . 2_665 ?
Na1 O7 H71 120.3 . . ?
Na1 O7 H71 110.4 2_665 . ?
Na1 O7 H72 87.7 . . ?
Na1 O7 H72 123.5 2_665 . ?
H71 O7 H72 108.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na1 O7 2.379(3) . ?
Na1 O2 2.387(3) . ?
Na1 O7 2.421(3) 3_565 ?
Na1 O6 2.480(4) . ?
Na1 O5 2.581(3) 18_554 ?
Na1 O3 2.815(3) 11_554 ?
Na1 As1 3.3634(16) 16_554 ?
Na1 Zn1 3.616(2) 16_554 ?
Na1 Na1 3.831(3) 2_665 ?
Na1 Na1 3.831(3) 3_565 ?
Na1 H61 2.4358 . ?
Na1 H72 2.5404 . ?
Zn1 O1 1.951(3) . ?
Zn1 O5 1.968(2) 2 ?
Zn1 O5 1.968(2) 3 ?
Zn1 O5 1.968(2) . ?
Zn1 Na1 3.616(2) 10_554 ?
Zn1 Na1 3.616(2) 11_444 ?
Zn1 Na1 3.616(2) 12_454 ?
Zn2 O2 1.946(2) . ?
Zn2 O3 1.959(2) . ?
Zn2 O4 1.961(2) . ?
Zn2 O1 1.9670(11) . ?
As1 O5 1.675(2) . ?
As1 O3 1.681(2) 11_554 ?
As1 O2 1.683(2) 10_554 ?
As1 O4 1.691(2) . ?
As1 Na1 3.3634(16) 10_554 ?
O1 Zn2 1.9670(11) 3 ?
O1 Zn2 1.9670(11) 2 ?
O2 As1 1.683(2) 16_554 ?
O3 As1 1.681(2) 17_544 ?
O3 Na1 2.815(3) 17_544 ?
O5 Na1 2.581(3) 12_454 ?
O6 H61 0.9039 . ?
O6 H62 0.8678 . ?
O7 Na1 2.421(3) 2_665 ?
O7 H71 0.9327 . ?
O7 H72 0.9940 . ?
