data_nza2
_database_code_CSD                  174788

#
# CIF data for Na3Zn4O(AsO4)3.6H2O
#
# REVISED cif to accompany submission B110288E to J. Mater. Chem.
# by Yeates and Harrison 
#

_journal_coden_Cambridge      1145

_publ_requested_journal       'Journal of Materials Chemistry'

loop_
_publ_author_name
'Harrison, William T. A.'
'Yeates, Rachel M.'

_publ_contact_author_name     	'Dr William T A Harrison'  
_publ_contact_author_address 
;
Department of Chemistry
University of Aberdeen
Aberdeen
Scotland
AB24 3UE
UNITED KINGDOM
;

_publ_contact_author_email       'W.HARRISON@ABDN.AC.UK'

_publ_section_title		
;
Synthesis, Crystal Structure and Properties
of Na3Zn4O(AsO4)3·6H2O, a New Framework Zincoarsenate
;

_audit_creation_method            SHELXL-97
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             'Sodium zinc arsenate' 
_chemical_melting_point           'decomposes before melting' 
_chemical_formula_moiety          ? 
_chemical_formula_sum             'H12 As3 Na3 O19 Zn4' 
_chemical_formula_weight          871.31 


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' 

_symmetry_cell_setting            'trigonal' 
_symmetry_space_group_name_H-M    'R 3 c' 

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' 

_cell_length_a                    10.9493(5) 
_cell_length_b                    10.9493(5) 
_cell_length_c                    26.7099(13) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      2773.2(2) 
_cell_formula_units_Z             6 
_cell_measurement_temperature     298(2) 
_cell_measurement_reflns_used     3933 
_cell_measurement_theta_min       2.64 
_cell_measurement_theta_max       32.20 

_exptl_crystal_description        'cube' 
_exptl_crystal_colour             'colourless' 
_exptl_crystal_size_max           0.13 
_exptl_crystal_size_mid           0.13 
_exptl_crystal_size_min           0.13 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.130 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2496 
_exptl_absorpt_coefficient_mu     10.617 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.3390 
_exptl_absorpt_correction_T_max   0.3390 
_exptl_absorpt_process_details    'SADABS (Bruker, 1999)' 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       298(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker SMART1000'  
_diffrn_measurement_method        \w 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             7427 
_diffrn_reflns_av_R_equivalents   0.0358 
_diffrn_reflns_av_sigmaI/netI     0.0335 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        9 
_diffrn_reflns_limit_l_min        -40 
_diffrn_reflns_limit_l_max        39 
_diffrn_reflns_theta_min          2.63 
_diffrn_reflns_theta_max          32.51 
_reflns_number_total              2095 
_reflns_number_gt                 1954 
_reflns_threshold_expression      'I>2sigma(I)'

_computing_data_collection        'SMART (Bruker, 1999)' 
_computing_cell_refinement        'SMART (Bruker, 1999)' 
_computing_data_reduction         'SAINT (Bruker, 1999)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'ORTEP-3 (Farrugia, 1997)' 
_computing_publication_material   'SMART (Bruker, 1999)' 

_refine_special_details 
; 
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ are statistically about twice as large as those based on F, and R- 
factors based on ALL data will be even larger. 
; 

_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
'calc w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.023(11) 
_refine_ls_number_reflns          2095 
_refine_ls_number_parameters      88 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0239 
_refine_ls_R_factor_gt            0.0211 
_refine_ls_wR_factor_ref          0.0423 
_refine_ls_wR_factor_gt           0.0419 
_refine_ls_goodness_of_fit_ref    1.000 
_refine_ls_restrained_S_all       0.999 
_refine_ls_shift/su_max           0.014 
_refine_ls_shift/su_mean          0.002 

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_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
Na1 0.0348(9) 0.0349(8) 0.0439(9) 0.0168(7) -0.0001(7) 0.0055(7) 
Zn1 0.01239(16) 0.01239(16) 0.0123(2) 0.000 0.000 0.00619(8) 
Zn2 0.01202(15) 0.01177(15) 0.01265(13) 0.00022(13) 0.00010(11) 0.00614(12) 
As1 0.00996(13) 0.01322(12) 0.01315(11) 0.00064(12) 0.00240(9) 0.00430(11) 
O1 0.0121(9) 0.0121(9) 0.0148(16) 0.000 0.000 0.0060(5) 
O2 0.0231(11) 0.0130(10) 0.0194(10) 0.0003(8) 0.0068(8) 0.0074(9) 
O3 0.0350(13) 0.0160(10) 0.0162(9) -0.0009(8) -0.0060(9) 0.0153(10) 
O4 0.0204(11) 0.0269(11) 0.0154(9) 0.0063(8) 0.0064(8) 0.0153(9) 
O5 0.0119(9) 0.0218(11) 0.0255(11) 0.0083(8) 0.0030(8) 0.0081(9) 
O6 0.0430(17) 0.0264(14) 0.0476(19) -0.0037(12) 0.0089(14) 0.0043(13) 
O7 0.0331(14) 0.0388(15) 0.0303(13) 0.0012(11) 0.0033(10) 0.0175(12) 

_geom_special_details 
; 
All esds (except the esd in the dihedral angle between two l.s. planes) 
are estimated using the full covariance matrix.  The cell esds are taken 
into account individually in the estimation of esds in distances, angles 
and torsion angles; correlations between esds in cell parameters are only 
used when they are defined by crystal symmetry.  An approximate (isotropic) 
treatment of cell esds is used for estimating esds involving l.s. planes. 
; 

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 . ? 

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 . . ? 

_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              32.51 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.460 
_refine_diff_density_min   -0.492 
_refine_diff_density_rms    0.095 

# end of file