# 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