# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350

_publ_contact_author_name        'Dezhong Shen'
_publ_contact_author_address     
;
Department of Chemistry,Tsinghua University, Beijing 100084, China
;
_publ_contact_author_email       zhangwl81@gmail.com
_publ_contact_author_phone       86(10)62772351

_publ_section_title              
;
Crystal Growth and Optical properties of a Noncentrosymmetric Molybdenum Tellurite Na2Te3Mo3O16
;
loop_
_publ_author_name
;
Wenlin Zhang, Jianfeng Sun, Xiaoqing Wang, Guangqiu Shen, Dezhong Shen
;
_publ_author_address             
;
Department of Chemistry,Tsinghua University, Beijing 100084, China
;

data_zhangwl6
_database_code_depnum_ccdc_archive 'CCDC 868984'
#TrackingRef '- cif_for_CE-ART-12-2011-006658.txt'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Mo3 O16 Te3, 2(Na)'
_chemical_formula_sum            'Mo3 Na2 O16 Te3'
_chemical_formula_weight         972.60

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   I2
_symmetry_space_group_name_Hall  'I 2y'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'

_cell_length_a                   7.3130(15)
_cell_length_b                   11.236(2)
_cell_length_c                   8.2171(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.26(3)
_cell_angle_gamma                90.00
_cell_volume                     669.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    1583
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      32.6

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    4.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864
_exptl_absorpt_coefficient_mu    9.326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.371
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   DTABSCOR

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(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  'Rigaku AFC10'
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4261
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         32.56
_reflns_number_total             2129
_reflns_number_gt                2016
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'

_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^)+(0.0010P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00347(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_number_reflns         2129
_refine_ls_number_parameters     112
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0646
_refine_ls_wR_factor_gt          0.0641
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

_iucr_refine_instructions_details 
;
TITL ZhangWL6 in I2
CELL 0.71073 7.3130 11.2360 8.2171 90.000 97.265 90.000
ZERR 2.00 0.0015 0.0022 0.0016 0.000 0.030 0.000
LATT -2
SYMM -X, Y, -Z
SFAC O NA MO TE
UNIT 32 4 6 6

EQIV $1 -0.5+X, 0.5+Y, -0.5+Z
EQIV $2 0.5-X, 0.5+Y, 1.5-Z

L.S. 4
ACTA
BOND
FMAP 2
PLAN 10

ISOR 0.001 O1 O4 O5

BIND TE1 O5_$1
BIND TE1 O5_$2

WGHT 0.001000
EXTI 0.003475
FVAR 0.26664
TE1 4 0.000000 0.989626 0.500000 10.50000 0.00476 0.00332 =
0.00451 0.00000 -0.00172 0.00000
TE2 4 0.278883 0.826819 0.281093 11.00000 0.00527 0.00562 =
0.00307 0.00068 -0.00196 0.00033
MO1 3 0.500000 0.579001 0.500000 10.50000 0.00598 0.00401 =
0.00393 0.00000 -0.00029 0.00000
MO2 3 0.253636 0.740256 0.727489 11.00000 0.00536 0.00488 =
0.00410 0.00028 -0.00068 0.00088
NA1 2 0.500000 1.071790 0.500000 10.50000 0.00722 0.01120 =
0.05626 0.00000 -0.01297 0.00000
NA2 2 0.500000 0.977097 0.000000 10.50000 0.00900 0.01080 =
0.01255 0.00000 0.00475 0.00000
O1 1 0.091881 0.877853 0.664276 11.00000 0.00775 0.00854 =
0.00714 0.00045 0.00028 0.00019
O2 1 0.242097 0.967546 0.402056 11.00000 0.00329 0.01296 =
0.00673 0.00034 0.00028 -0.00098
O3 1 0.311138 0.730308 0.472284 11.00000 0.00599 0.00986 =
0.00310 0.00057 -0.00207 0.00211
O4 1 0.520028 0.869251 0.262513 11.00000 0.00615 0.00676 =
0.00748 0.00063 0.00014 -0.00038
O5 1 0.458244 0.626500 0.717847 11.00000 0.00609 0.00571 =
0.00632 0.00033 -0.00004 0.00097
O6 1 0.185884 0.984285 0.049364 11.00000 0.01285 0.00544 =
0.00800 0.00002 0.00139 0.00111
O7 1 0.271827 0.746432 0.936939 11.00000 0.01577 0.01595 =
0.00893 0.00012 0.00101 0.00718
O8 1 0.080161 0.637499 0.691387 11.00000 0.01248 0.01339 =
0.01316 -0.00425 0.00129 -0.00239
HKLF 4

REM ZhangWL6 in I2
REM R1 = 0.0292 for 2016 Fo > 4sig(Fo) and 0.0307 for all 2129 data
REM 112 parameters refined using 19 restraints

END
;

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
Te1 Te 0.0000 0.98963(6) 0.5000 0.00439(17) Uani 1 2 d S . .
Te2 Te 0.27888(6) 0.82682(5) 0.28109(6) 0.00487(12) Uani 1 1 d . . .
Mo1 Mo 0.5000 0.57900(10) 0.5000 0.0047(2) Uani 1 2 d S . .
Mo2 Mo 0.25364(12) 0.74026(5) 0.72749(8) 0.00489(16) Uani 1 1 d . . .
Na1 Na 0.5000 1.0718(7) 0.5000 0.0263(19) Uani 1 2 d S . .
Na2 Na 0.5000 0.9771(5) 0.0000 0.0105(12) Uani 1 2 d S . .
O1 O 0.0919(7) 0.8779(4) 0.6643(6) 0.0079(10) Uani 1 1 d U . .
O2 O 0.2421(7) 0.9675(5) 0.4021(7) 0.0077(11) Uani 1 1 d . . .
O3 O 0.3111(7) 0.7303(5) 0.4723(6) 0.0065(10) Uani 1 1 d . . .
O4 O 0.5200(7) 0.8693(4) 0.2625(6) 0.0069(11) Uani 1 1 d U . .
O5 O 0.4582(7) 0.6265(4) 0.7178(6) 0.0061(10) Uani 1 1 d U . .
O6 O 0.1859(7) 0.9843(5) 0.0494(6) 0.0088(11) Uani 1 1 d . . .
O7 O 0.2718(8) 0.7464(5) 0.9369(7) 0.0136(11) Uani 1 1 d . . .
O8 O 0.0802(8) 0.6375(5) 0.6914(7) 0.0130(12) Uani 1 1 d . . .

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
Te1 0.0048(3) 0.0033(3) 0.0045(4) 0.000 -0.0017(3) 0.000
Te2 0.0053(2) 0.0056(2) 0.0031(2) 0.0007(2) -0.00196(15) 0.0003(2)
Mo1 0.0060(6) 0.0040(5) 0.0039(6) 0.000 -0.0003(4) 0.000
Mo2 0.0054(3) 0.0049(3) 0.0041(4) 0.0003(3) -0.0007(2) 0.0009(2)
Na1 0.007(3) 0.011(3) 0.056(6) 0.000 -0.013(3) 0.000
Na2 0.009(2) 0.011(3) 0.013(3) 0.000 0.005(2) 0.000
O1 0.0078(13) 0.0085(13) 0.0071(13) 0.0005(9) 0.0003(9) 0.0002(9)
O2 0.003(2) 0.013(3) 0.007(3) 0.000(2) 0.0003(19) -0.0010(19)
O3 0.006(2) 0.010(2) 0.003(2) 0.001(2) -0.0021(17) 0.002(2)
O4 0.0061(13) 0.0068(13) 0.0075(13) 0.0006(9) 0.0001(9) -0.0004(9)
O5 0.0061(13) 0.0057(13) 0.0063(13) 0.0003(9) 0.0000(9) 0.0010(9)
O6 0.013(3) 0.005(3) 0.008(3) 0.000(2) 0.001(2) 0.001(2)
O7 0.016(3) 0.016(3) 0.009(3) 0.000(2) 0.001(2) 0.007(2)
O8 0.012(3) 0.013(3) 0.013(3) -0.004(2) 0.001(2) -0.002(2)

_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
Te1 O1 1.903(5) . ?
Te1 O1 1.903(5) 2_556 ?
Te1 O2 2.050(5) . ?
Te1 O2 2.050(5) 2_556 ?
Te1 O5 2.767(5) 4_556 ?
Te1 O5 2.767(5) 3_454 ?
Te2 O4 1.852(5) . ?
Te2 O3 1.899(5) . ?
Te2 O2 1.905(5) . ?
Mo1 O6 1.734(5) 4_545 ?
Mo1 O6 1.734(5) 3_545 ?
Mo1 O5 1.929(5) . ?
Mo1 O5 1.929(5) 2_656 ?
Mo1 O3 2.184(5) 2_656 ?
Mo1 O3 2.184(5) . ?
Mo2 O7 1.711(6) . ?
Mo2 O8 1.713(6) . ?
Mo2 O1 1.976(5) . ?
Mo2 O5 1.977(5) . ?
Mo2 O3 2.193(5) . ?
Mo2 O4 2.194(5) 2_656 ?
Na1 O2 2.279(7) . ?
Na1 O2 2.279(7) 2_656 ?
Na1 O8 2.774(6) 4_556 ?
Na1 O8 2.774(6) 3_554 ?
Na1 O7 2.886(8) 3_554 ?
Na1 O7 2.886(8) 4_556 ?
Na1 O4 3.013(8) 2_656 ?
Na1 O4 3.013(8) . ?
Na2 O6 2.384(5) . ?
Na2 O6 2.384(5) 2_655 ?
Na2 O8 2.415(7) 3_554 ?
Na2 O8 2.415(7) 4 ?
Na2 O4 2.462(6) 2_655 ?
Na2 O4 2.462(6) . ?
O4 Mo2 2.194(5) 2_656 ?
O6 Mo1 1.734(5) 3_454 ?
O7 Na1 2.886(8) 3_445 ?
O8 Na2 2.415(7) 3_445 ?
O8 Na1 2.774(6) 3_445 ?

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 Te1 O1 97.4(3) . 2_556 ?
O1 Te1 O2 87.3(2) . . ?
O1 Te1 O2 83.5(2) 2_556 . ?
O1 Te1 O2 83.5(2) . 2_556 ?
O1 Te1 O2 87.3(2) 2_556 2_556 ?
O2 Te1 O2 166.1(3) . 2_556 ?
O1 Te1 O5 77.34(18) . 4_556 ?
O1 Te1 O5 162.35(18) 2_556 4_556 ?
O2 Te1 O5 112.76(18) . 4_556 ?
O2 Te1 O5 75.38(18) 2_556 4_556 ?
O1 Te1 O5 162.35(18) . 3_454 ?
O1 Te1 O5 77.34(18) 2_556 3_454 ?
O2 Te1 O5 75.38(18) . 3_454 ?
O2 Te1 O5 112.76(18) 2_556 3_454 ?
O5 Te1 O5 112.5(2) 4_556 3_454 ?
O4 Te2 O3 101.3(2) . . ?
O4 Te2 O2 91.6(2) . . ?
O3 Te2 O2 93.1(2) . . ?
O6 Mo1 O6 104.3(4) 4_545 3_545 ?
O6 Mo1 O5 100.1(2) 4_545 . ?
O6 Mo1 O5 99.5(2) 3_545 . ?
O6 Mo1 O5 99.5(2) 4_545 2_656 ?
O6 Mo1 O5 100.1(2) 3_545 2_656 ?
O5 Mo1 O5 147.9(3) . 2_656 ?
O6 Mo1 O3 165.7(2) 4_545 2_656 ?
O6 Mo1 O3 89.2(2) 3_545 2_656 ?
O5 Mo1 O3 82.0(2) . 2_656 ?
O5 Mo1 O3 73.1(2) 2_656 2_656 ?
O6 Mo1 O3 89.2(2) 4_545 . ?
O6 Mo1 O3 165.7(2) 3_545 . ?
O5 Mo1 O3 73.1(2) . . ?
O5 Mo1 O3 82.0(2) 2_656 . ?
O3 Mo1 O3 77.8(3) 2_656 . ?
O7 Mo2 O8 99.4(3) . . ?
O7 Mo2 O1 101.6(2) . . ?
O8 Mo2 O1 94.4(2) . . ?
O7 Mo2 O5 95.9(2) . . ?
O8 Mo2 O5 96.0(2) . . ?
O1 Mo2 O5 157.9(2) . . ?
O7 Mo2 O3 164.6(2) . . ?
O8 Mo2 O3 91.6(2) . . ?
O1 Mo2 O3 88.2(2) . . ?
O5 Mo2 O3 72.0(2) . . ?
O7 Mo2 O4 88.5(2) . 2_656 ?
O8 Mo2 O4 172.0(2) . 2_656 ?
O1 Mo2 O4 85.2(2) . 2_656 ?
O5 Mo2 O4 81.80(18) . 2_656 ?
O3 Mo2 O4 80.5(2) . 2_656 ?
O2 Na1 O2 118.1(4) . 2_656 ?
O2 Na1 O8 101.45(18) . 4_556 ?
O2 Na1 O8 94.31(17) 2_656 4_556 ?
O2 Na1 O8 94.31(17) . 3_554 ?
O2 Na1 O8 101.45(18) 2_656 3_554 ?
O8 Na1 O8 149.1(4) 4_556 3_554 ?
O2 Na1 O7 147.6(2) . 3_554 ?
O2 Na1 O7 81.65(17) 2_656 3_554 ?
O8 Na1 O7 102.3(3) 4_556 3_554 ?
O8 Na1 O7 54.90(18) 3_554 3_554 ?
O2 Na1 O7 81.65(17) . 4_556 ?
O2 Na1 O7 147.6(2) 2_656 4_556 ?
O8 Na1 O7 54.90(18) 4_556 4_556 ?
O8 Na1 O7 102.3(3) 3_554 4_556 ?
O7 Na1 O7 94.3(3) 3_554 4_556 ?
O2 Na1 O4 74.6(3) . 2_656 ?
O2 Na1 O4 59.3(2) 2_656 2_656 ?
O8 Na1 O4 64.90(15) 4_556 2_656 ?
O8 Na1 O4 145.7(3) 3_554 2_656 ?
O7 Na1 O4 136.11(15) 3_554 2_656 ?
O7 Na1 O4 107.83(14) 4_556 2_656 ?
O2 Na1 O4 59.3(2) . . ?
O2 Na1 O4 74.6(3) 2_656 . ?
O8 Na1 O4 145.7(3) 4_556 . ?
O8 Na1 O4 64.90(15) 3_554 . ?
O7 Na1 O4 107.83(14) 3_554 . ?
O7 Na1 O4 136.11(15) 4_556 . ?
O4 Na1 O4 81.9(3) 2_656 . ?
O6 Na2 O6 176.1(4) . 2_655 ?
O6 Na2 O8 91.4(2) . 3_554 ?
O6 Na2 O8 85.7(2) 2_655 3_554 ?
O6 Na2 O8 85.7(2) . 4 ?
O6 Na2 O8 91.4(2) 2_655 4 ?
O8 Na2 O8 83.5(3) 3_554 4 ?
O6 Na2 O4 102.35(19) . 2_655 ?
O6 Na2 O4 79.60(17) 2_655 2_655 ?
O8 Na2 O4 157.0(2) 3_554 2_655 ?
O8 Na2 O4 79.29(18) 4 2_655 ?
O6 Na2 O4 79.60(17) . . ?
O6 Na2 O4 102.35(19) 2_655 . ?
O8 Na2 O4 79.29(18) 3_554 . ?
O8 Na2 O4 157.0(2) 4 . ?
O4 Na2 O4 121.0(3) 2_655 . ?
Te1 O1 Mo2 148.1(3) . . ?
Te2 O2 Te1 119.4(2) . . ?
Te2 O2 Na1 116.5(3) . . ?
Te1 O2 Na1 121.1(3) . . ?
Te2 O3 Mo1 122.8(2) . . ?
Te2 O3 Mo2 138.0(3) . . ?
Mo1 O3 Mo2 97.8(2) . . ?
Te2 O4 Mo2 123.3(2) . 2_656 ?
Te2 O4 Na2 104.3(2) . . ?
Mo2 O4 Na2 108.6(2) 2_656 . ?
Te2 O4 Na1 90.93(18) . . ?
Mo2 O4 Na1 125.0(2) 2_656 . ?
Na2 O4 Na1 101.1(3) . . ?
Mo1 O5 Mo2 115.2(3) . . ?
Mo1 O6 Na2 136.5(3) 3_454 . ?
Mo2 O7 Na1 100.7(2) . 3_445 ?
Mo2 O8 Na2 136.8(3) . 3_445 ?
Mo2 O8 Na1 105.0(3) . 3_445 ?
Na2 O8 Na1 109.6(3) 3_445 3_445 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        32.56
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.429
_refine_diff_density_min         -2.605
_refine_diff_density_rms         0.345