# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Prof. Jingping Wang'
_publ_contact_author_email       jpwang@henu.edu.cn

_publ_section_title              
;
A Novel Organic-Inorganic Hybrid
Turbine-Shaped Hexa-Zn Sandwiched Tungstoarsenate(III)

;
loop_
_publ_author_name
'Jingping Wang'
'Jingyang Niu'
'Xiang Ma'
'Junwei Zhao'
'Pengtao Ma'
;
Chao Zhang
;

# Attachment '- 1.cif'

data_njy1
_database_code_depnum_ccdc_archive 'CCDC 818189'
#TrackingRef '- 1.cif'

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            'C12 H66 As2 N12 O72 W18 Zn6'

_chemical_formula_weight         5382.13

loop_

_atom_type_symbol

_atom_type_description

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_source

C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Rhombohedral

_symmetry_space_group_name_H-M   R-3

loop_

_symmetry_equiv_pos_as_xyz

'x, y, z'
'z, x, y'
'y, z, x'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'

_cell_length_a                   13.175(4)

_cell_length_b                   13.175(4)

_cell_length_c                   13.175(4)

_cell_angle_alpha                104.00

_cell_angle_beta                 104.00

_cell_angle_gamma                104.00

_cell_volume                     2040.8(10)

_cell_formula_units_Z            1

_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    447

_cell_measurement_theta_min      2.73

_cell_measurement_theta_max      19.10

_exptl_crystal_description       block

_exptl_crystal_colour            colorless

_exptl_crystal_size_max          0.18

_exptl_crystal_size_mid          0.11

_exptl_crystal_size_min          0.08

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    4.379

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             2376

_exptl_absorpt_coefficient_mu    27.888

_exptl_absorpt_correction_type   Multi-scan

_exptl_absorpt_correction_T_min  0.0817

_exptl_absorpt_correction_T_max  0.2138

_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;

?

;

_diffrn_ambient_temperature      296(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  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            10301

_diffrn_reflns_av_R_equivalents  0.0508

_diffrn_reflns_av_sigmaI/netI    0.0461

_diffrn_reflns_limit_h_min       -14

_diffrn_reflns_limit_h_max       15

_diffrn_reflns_limit_k_min       -11

_diffrn_reflns_limit_k_max       15

_diffrn_reflns_limit_l_min       -12

_diffrn_reflns_limit_l_max       15

_diffrn_reflns_theta_min         1.96

_diffrn_reflns_theta_max         25.00

_reflns_number_total             2383

_reflns_number_gt                1942

_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'

_computing_cell_refinement       'Bruker SMART'

_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    'Bruker SHELXTL'

_computing_publication_material  'Bruker SHELXTL'

_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. O2, O1W and O2W are restrained
by the ISOR instruction because they are ADP or NDP alerts.

;

_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^)+(0.0499P)^2^+40.7117P] 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    constr

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_number_reflns         2383

_refine_ls_number_parameters     193

_refine_ls_number_restraints     18

_refine_ls_R_factor_all          0.0557

_refine_ls_R_factor_gt           0.0405

_refine_ls_wR_factor_ref         0.1069

_refine_ls_wR_factor_gt          0.0997

_refine_ls_goodness_of_fit_ref   1.072

_refine_ls_restrained_S_all      1.085

_refine_ls_shift/su_max          0.000

_refine_ls_shift/su_mean         0.000

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

W1 W 0.26163(5) 0.10343(5) 0.06924(5) 0.0249(2) Uani 1 1 d . . .
W2 W 0.49769(5) 0.16497(5) 0.27844(5) 0.02453(19) Uani 1 1 d . . .
W3 W 0.33914(5) 0.13243(5) 0.47057(5) 0.02416(19) Uani 1 1 d . . .
As1 As 0.33763(15) 0.33763(15) 0.33763(15) 0.0181(5) Uani 1 3 d S . .
Zn1 Zn 0.43794(14) 0.39269(13) 0.67288(14) 0.0242(4) Uani 1 1 d . . .
O1 O 0.2071(10) -0.0077(10) -0.0494(9) 0.043(3) Uani 1 1 d . . .
O2 O 0.1727(7) 0.1964(7) 0.0398(8) 0.019(2) Uani 1 1 d U . .
O3 O 0.3610(8) 0.2014(9) 0.0264(8) 0.029(2) Uani 1 1 d . . .
O4 O 0.3809(9) 0.0612(9) 0.1446(8) 0.029(2) Uani 1 1 d . . .
O5 O 0.3694(8) 0.2521(8) 0.2284(8) 0.022(2) Uani 1 1 d . . .
O6 O 0.5469(9) 0.2413(9) 0.1829(9) 0.032(2) Uani 1 1 d . . .
O7 O 0.5884(9) 0.0904(9) 0.2880(9) 0.035(3) Uani 1 1 d . . .
O8 O 0.5685(8) 0.2939(8) 0.3957(8) 0.026(2) Uani 1 1 d . . .
O9 O 0.4091(8) 0.1102(9) 0.3604(8) 0.030(2) Uani 1 1 d . . .
O10 O 0.4440(8) 0.2695(8) 0.5485(8) 0.027(2) Uani 1 1 d . . .
O11 O 0.3754(10) 0.0465(9) 0.5403(9) 0.038(3) Uani 1 1 d . . .
C1 C 0.3057(15) 0.3612(14) 0.8242(15) 0.042(4) Uani 1 1 d . . .
H1A H 0.2728 0.3969 0.7749 0.050 Uiso 1 1 calc R . .
H1B H 0.3281 0.4103 0.8993 0.050 Uiso 1 1 calc R . .
C2 C 0.2223(17) 0.2550(18) 0.8117(18) 0.057(5) Uani 1 1 d . . .
H2A H 0.2047 0.2035 0.7386 0.068 Uiso 1 1 calc R . .
H2B H 0.2530 0.2226 0.8655 0.068 Uiso 1 1 calc R . .
N1 N 0.4040(12) 0.3403(12) 0.7984(11) 0.040(3) Uani 1 1 d . . .
H1C H 0.3937 0.2673 0.7806 0.048 Uiso 1 1 calc R . .
H1D H 0.4632 0.3741 0.8595 0.048 Uiso 1 1 calc R . .
N2 N 0.1202(16) 0.2747(17) 0.8278(17) 0.080(7) Uani 1 1 d . . .
H2C H 0.0715 0.2110 0.8199 0.121 Uiso 1 1 calc R . .
H2D H 0.0917 0.3038 0.7779 0.121 Uiso 1 1 calc R . .
H2E H 0.1363 0.3210 0.8953 0.121 Uiso 1 1 calc R . .
O1W O 0.621(3) -0.112(3) 0.215(3) 0.082(10) Uani 0.50 1 d PU . .
O2W O 0.466(3) -0.099(3) 0.038(3) 0.100(12) Uani 0.50 1 d PU . .

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

W1 0.0251(3) 0.0220(3) 0.0219(3) 0.0019(3) 0.0055(3) 0.0048(3)
W2 0.0213(3) 0.0224(3) 0.0255(3) 0.0032(2) 0.0036(3) 0.0074(2)
W3 0.0232(3) 0.0215(3) 0.0238(3) 0.0078(2) 0.0029(2) 0.0043(2)
As1 0.0171(6) 0.0171(6) 0.0171(6) 0.0037(7) 0.0037(7) 0.0037(7)
Zn1 0.0241(9) 0.0227(9) 0.0261(9) 0.0082(7) 0.0083(7) 0.0073(7)
O1 0.050(8) 0.036(7) 0.026(6) -0.011(5) 0.009(5) 0.007(6)
O2 0.016(3) 0.018(3) 0.018(3) -0.0049(18) -0.0023(18) 0.0147(19)
O3 0.028(6) 0.029(6) 0.023(6) 0.002(4) 0.011(5) -0.002(5)
O4 0.029(6) 0.025(6) 0.027(6) 0.004(4) 0.004(5) 0.006(5)
O5 0.016(5) 0.019(5) 0.025(5) 0.002(4) 0.003(4) 0.002(4)
O6 0.036(6) 0.029(6) 0.030(6) 0.006(5) 0.010(5) 0.013(5)
O7 0.036(6) 0.031(6) 0.038(7) 0.012(5) 0.004(5) 0.019(5)
O8 0.025(6) 0.031(6) 0.017(5) 0.006(4) 0.003(4) 0.004(4)
O9 0.025(6) 0.040(6) 0.026(6) 0.010(5) 0.015(5) 0.007(5)
O10 0.018(5) 0.027(6) 0.026(6) 0.000(4) 0.003(4) 0.001(4)
O11 0.046(7) 0.037(7) 0.033(6) 0.017(5) 0.003(5) 0.019(6)
C1 0.055(12) 0.027(9) 0.045(11) 0.006(8) 0.033(9) 0.004(8)
C2 0.054(13) 0.055(13) 0.052(13) 0.027(10) 0.007(10) 0.002(10)
N1 0.046(9) 0.036(8) 0.034(8) 0.012(6) 0.013(7) 0.006(7)
N2 0.074(14) 0.072(13) 0.066(13) -0.007(10) 0.038(11) -0.015(11)
O1W 0.095(13) 0.073(12) 0.086(13) 0.022(9) 0.039(9) 0.035(9)
O2W 0.100(14) 0.100(15) 0.103(15) 0.016(9) 0.035(10) 0.048(10)

_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

W1 O1 1.716(10) . ?
W1 O3 1.895(10) . ?
W1 O4 1.924(10) . ?
W1 O2 1.930(8) . ?
W1 O2 2.018(8) 3 ?
W1 O5 2.341(9) . ?
W2 O7 1.722(10) . ?
W2 O8 1.847(10) . ?
W2 O9 1.905(9) . ?
W2 O6 1.925(11) . ?
W2 O4 1.962(10) . ?
W2 O5 2.319(9) . ?
W3 O11 1.705(10) . ?
W3 O10 1.853(10) . ?
W3 O9 1.901(9) . ?
W3 O6 1.958(10) 3 ?
W3 O3 1.965(10) 3 ?
W3 O5 2.338(10) 3 ?
As1 O5 1.803(10) 2 ?
As1 O5 1.803(10) . ?
As1 O5 1.803(10) 3 ?
Zn1 O8 2.035(10) 5_666 ?
Zn1 O10 2.042(10) . ?
Zn1 N1 2.042(13) . ?
Zn1 O10 2.048(10) 5_666 ?
Zn1 O8 2.072(10) 3 ?
Zn1 Zn1 3.1236(19) 5_666 ?
Zn1 Zn1 3.1236(19) 6_666 ?
O2 W1 2.018(8) 2 ?
O3 W3 1.965(10) 2 ?
O5 W3 2.338(10) 2 ?
O6 W3 1.958(10) 2 ?
O8 Zn1 2.035(10) 6_666 ?
O8 Zn1 2.072(10) 2 ?
O10 Zn1 2.048(10) 6_666 ?
C1 N1 1.49(2) . ?
C1 C2 1.50(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.48(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
N1 H1C 0.9000 . ?
N1 H1D 0.9000 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?

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

O1 W1 O3 100.2(5) . . ?
O1 W1 O4 98.7(5) . . ?
O3 W1 O4 90.3(5) . . ?
O1 W1 O2 102.8(5) . . ?
O3 W1 O2 82.2(5) . . ?
O4 W1 O2 158.2(4) . . ?
O1 W1 O2 100.9(5) . 3 ?
O3 W1 O2 157.5(4) . 3 ?
O4 W1 O2 78.9(4) . 3 ?
O2 W1 O2 100.5(6) . 3 ?
O1 W1 O5 168.7(5) . . ?
O3 W1 O5 73.2(4) . . ?
O4 W1 O5 72.6(4) . . ?
O2 W1 O5 85.6(4) . . ?
O2 W1 O5 84.7(3) 3 . ?
O7 W2 O8 104.4(5) . . ?
O7 W2 O9 100.9(5) . . ?
O8 W2 O9 89.8(4) . . ?
O7 W2 O6 98.6(5) . . ?
O8 W2 O6 89.1(4) . . ?
O9 W2 O6 160.2(4) . . ?
O7 W2 O4 98.7(5) . . ?
O8 W2 O4 156.9(4) . . ?
O9 W2 O4 87.3(4) . . ?
O6 W2 O4 86.1(4) . . ?
O7 W2 O5 168.7(4) . . ?
O8 W2 O5 84.5(4) . . ?
O9 W2 O5 86.1(4) . . ?
O6 W2 O5 74.2(4) . . ?
O4 W2 O5 72.5(4) . . ?
O11 W3 O10 105.0(5) . . ?
O11 W3 O9 101.5(5) . . ?
O10 W3 O9 91.4(5) . . ?
O11 W3 O6 100.0(5) . 3 ?
O10 W3 O6 87.3(4) . 3 ?
O9 W3 O6 158.1(5) . 3 ?
O11 W3 O3 97.9(5) . 3 ?
O10 W3 O3 156.6(4) . 3 ?
O9 W3 O3 88.4(5) . 3 ?
O6 W3 O3 84.3(5) 3 3 ?
O11 W3 O5 168.1(5) . 3 ?
O10 W3 O5 84.6(4) . 3 ?
O9 W3 O5 85.0(4) . 3 ?
O6 W3 O5 73.1(4) 3 3 ?
O3 W3 O5 72.1(4) 3 3 ?
O5 As1 O5 97.7(4) 2 . ?
O5 As1 O5 97.7(4) 2 3 ?
O5 As1 O5 97.7(4) . 3 ?
O8 Zn1 O10 80.1(4) 5_666 . ?
O8 Zn1 N1 106.0(5) 5_666 . ?
O10 Zn1 N1 112.9(5) . . ?
O8 Zn1 O10 91.1(4) 5_666 5_666 ?
O10 Zn1 O10 146.5(6) . 5_666 ?
N1 Zn1 O10 100.6(5) . 5_666 ?
O8 Zn1 O8 144.4(6) 5_666 3 ?
O10 Zn1 O8 89.4(4) . 3 ?
N1 Zn1 O8 109.3(5) . 3 ?
O10 Zn1 O8 79.1(4) 5_666 3 ?
O8 Zn1 Zn1 117.7(3) 5_666 5_666 ?
O10 Zn1 Zn1 117.6(3) . 5_666 ?
N1 Zn1 Zn1 116.7(4) . 5_666 ?
O10 Zn1 Zn1 40.1(3) 5_666 5_666 ?
O8 Zn1 Zn1 40.1(3) 3 5_666 ?
O8 Zn1 Zn1 40.9(3) 5_666 6_666 ?
O10 Zn1 Zn1 40.3(3) . 6_666 ?
N1 Zn1 Zn1 123.1(4) . 6_666 ?
O10 Zn1 Zn1 119.2(3) 5_666 6_666 ?
O8 Zn1 Zn1 116.4(3) 3 6_666 ?
Zn1 Zn1 Zn1 119.985(3) 5_666 6_666 ?
W1 O2 W1 138.4(5) . 2 ?
W1 O3 W3 122.2(5) . 2 ?
W1 O4 W2 121.4(5) . . ?
As1 O5 W2 117.5(5) . . ?
As1 O5 W3 118.0(5) . 2 ?
W2 O5 W3 92.4(3) . 2 ?
As1 O5 W1 133.5(5) . . ?
W2 O5 W1 93.3(3) . . ?
W3 O5 W1 92.5(3) 2 . ?
W2 O6 W3 119.9(5) . 2 ?
W2 O8 Zn1 132.7(5) . 6_666 ?
W2 O8 Zn1 126.1(5) . 2 ?
Zn1 O8 Zn1 99.0(4) 6_666 2 ?
W3 O9 W2 151.5(6) . . ?
W3 O10 Zn1 128.4(5) . . ?
W3 O10 Zn1 130.7(5) . 6_666 ?
Zn1 O10 Zn1 99.6(4) . 6_666 ?
N1 C1 C2 110.5(15) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C1 110.5(18) . . ?
N2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C1 N1 Zn1 114.6(11) . . ?
C1 N1 H1C 108.6 . . ?
Zn1 N1 H1C 108.6 . . ?
C1 N1 H1D 108.6 . . ?
Zn1 N1 H1D 108.6 . . ?
H1C N1 H1D 107.6 . . ?
C2 N2 H2C 109.5 . . ?
C2 N2 H2D 109.5 . . ?
H2C N2 H2D 109.5 . . ?
C2 N2 H2E 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?

loop_

_geom_hbond_atom_site_label_D

_geom_hbond_atom_site_label_H

_geom_hbond_atom_site_label_A

_geom_hbond_distance_DH

_geom_hbond_distance_HA

_geom_hbond_distance_DA

_geom_hbond_angle_DHA

_geom_hbond_site_symmetry_A

N1 H1C O1W 0.90 2.02 2.90(4) 164.7 4_656
N1 H1D O11 0.90 2.42 3.186(18) 143.0 2_556
N2 H2C O1 0.89 2.00 2.85(2) 159.0 6_556
N2 H2D O7 0.89 2.45 3.14(2) 134.1 3
N2 H2E O4 0.89 2.10 2.96(2) 160.5 2_556
N2 H2E O2W 0.89 2.54 3.01(5) 113.6 2_556

_diffrn_measured_fraction_theta_max 0.990

_diffrn_reflns_theta_full        25.00

_diffrn_measured_fraction_theta_full 0.990

_refine_diff_density_max         4.278

_refine_diff_density_min         -1.854

_refine_diff_density_rms         0.342