Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 1145 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name J.Gopalakrishnan Y.Piffard 'Litty, Sebastian' A.K.Shukla F.Taulelle _publ_contact_author_name 'Prof J. Gopalakrishnan' _publ_contact_author_address ; Prof J. Gopalakrishnan Solid State and Structural Chemistry Unit Indian Institute of Science C.V.Raman Avenue Bangalore Karnataka 560012 INDIA ; _publ_contact_author_email GOPAL@SSCU.IISC.ERNET.IN _publ_section_title ; Synthesis, structure and lithium-ion conductivity of Li2-2xMg2+x(MoO4)3 and Li3M(MoO4)3 (MIII = Cr, Fe) ; data_Li2Mg2(MoO4)3 _database_code_CSD 207253 _cell_length_a 5.1167 _cell_length_b 10.4646 _cell_length_c 17.6228 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 943.599 _cell_measurement_pressure normal _cell_measurement_radiation 'Cu K\a1' _cell_measurement_reflns_used 'full pattern matching' _cell_measurement_temperature 293 _cell_measurement_theta_max 114.6 _cell_measurement_theta_min 8.0 _cell_measurement_wavelength 1.540598 _cell_formula_units_Z 4 _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number Pnma loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,y,1/2-z 3 1/2-x,1/2+y,1/2+z 4 -x,1/2+y,-z 5 -x,-y,-z 6 1/2-x,-y,1/2+z 7 1/2+x,1/2-y,1/2-z 8 x,1/2-y,z loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_versus_stol_list Li 0 16 0.000 0.000 International_Tables_Vol_C ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 3.000 2.708 2.214 1.904 1.742 1.625 1.511 1.393 1.271 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 1.151 1.035 0.925 0.823 0.731 0.648 0.575 0.510 0.453 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 0.404 0.360 0.321 0.287 0.257 0.230 0.206 0.185 0.166 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 0.149 0.134 0.120 0.108 0.098 0.088 0.081 0.074 0.068 stol 1.80 1.85 1.90 1.95 2.00 2.05 2.10 2.15 2.20 f 0.063 0.058 0.055 0.051 0.049 0.047 0.045 0.043 0.042 stol 2.25 2.30 2.35 2.40 2.45 2.50 2.55 2.60 2.65 f 0.041 0.041 0.040 0.039 0.039 0.039 0.039 0.038 0.038 ; O 0 96 0.011 0.006 International_Tables_Vol_C ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 8.000 7.798 7.246 6.472 5.623 4.808 4.089 3.489 3.006 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 2.628 2.337 2.115 1.946 1.816 1.715 1.634 1.568 1.512 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 1.463 1.419 1.377 1.337 1.298 1.260 1.221 1.183 1.145 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 1.108 1.070 1.033 0.997 0.961 0.926 0.891 0.857 0.824 stol 1.80 1.85 1.90 1.95 2.00 2.05 2.10 2.15 2.20 f 0.792 0.761 0.731 0.702 0.674 0.647 0.621 0.597 0.573 stol 2.25 2.30 2.35 2.40 2.45 2.50 2.55 2.60 2.65 f 0.551 0.530 0.509 0.490 0.472 0.455 0.439 0.424 0.410 ; Mg 0 16 0.049 0.036 International_Tables_Vol_C ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 12.000 11.515 10.481 9.489 8.729 8.086 7.456 6.819 6.191 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 5.589 5.029 4.518 4.060 3.655 3.301 2.994 2.730 2.506 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 2.315 2.154 2.019 1.905 1.810 1.729 1.660 1.601 1.549 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 1.503 1.461 1.424 1.389 1.356 1.325 1.296 1.268 1.242 stol 1.80 1.85 1.90 1.95 2.00 2.05 2.10 2.15 2.20 f 1.216 1.192 1.169 1.147 1.126 1.106 1.087 1.069 1.053 stol 2.25 2.30 2.35 2.40 2.45 2.50 2.55 2.60 2.65 f 1.037 1.022 1.008 0.995 0.983 0.972 0.962 0.952 0.943 ; Mo 0 24 -1.683 0.686 International_Tables_Vol_C ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 42.000 41.022 38.693 35.879 33.162 30.679 28.417 26.387 24.609 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 23.082 21.771 20.627 19.601 18.652 17.753 16.887 16.047 15.231 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 14.442 13.682 12.955 12.264 11.612 11.000 10.429 9.899 9.410 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 8.961 8.550 8.176 7.836 7.529 7.251 7.001 6.776 6.573 stol 1.80 1.85 1.90 1.95 2.00 2.05 2.10 2.15 2.20 f 6.391 6.226 6.079 5.945 5.824 5.715 5.615 5.524 5.441 stol 2.25 2.30 2.35 2.40 2.45 2.50 2.55 2.60 2.65 f 5.365 5.294 5.229 5.169 5.113 5.061 5.012 4.966 4.924 ; _chemical_formula_sum 'Li2 O12 Mg2 Mo3' _chemical_formula_weight 539.3 _exptl_crystal_colour colorless _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.045 _exptl_crystal_size_min 0.045 _exptl_crystal_size_rad ? _exptl_crystal_density_meas 3.798 _exptl_crystal_density_meas_temp ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1008 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 1.000 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_coefficient_mu 4.122 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type CAD4 _diffrn_measurement_method \q/2\q _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_standards_number 3 _diffrn_standards_decay_% 0.2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 4 0 1 5 3 1 -5 3 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 30 _reflns_limit_h_min 0 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _diffrn_reflns_number 3472 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 37.93 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0474 _reflns_observed_criterion 3 _reflns_number_total 2645 _reflns_number_observed 1740 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/\s^2^(F) _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_gt 0.0240 _refine_ls_R_factor_all 0.0660 _refine_ls_wR_factor_all 0.0251 _refine_ls_number_reflns 2645 _refine_ls_number_parameters 85 _refine_ls_goodness_of_fit_all 1.70 _refine_ls_goodness_of_fit_obs 1.43 _refine_ls_shift/esd_max 0.0006 _refine_ls_shift/esd_mean 0.0001 _refine_diff_density_max 2.60 _refine_diff_density_min -2.35 _refine_ls_extinction_method 'B-C type 1 Lorentzian isotropic' _refine_ls_extinction_coef 0.026(1) loop_ _atom_site_label _atom_site_type_symbol _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Mo1 Mo 2 1 0.22044(7) 0.25 0.05688(2) 0.00721(7) Mo2 Mo 1 1 0.27554(5) 0.02686(2) 0.84338(1) 0.00811(5) Mg1 Mg 1 0.659(3) 0.7529(3) 0.0750(1) 0.97230(6) 0.0099(2) Li1 Li 1 0.341(3) 0.7529(3) 0.0750(1) 0.97230(6) 0.0099(2) Mg2 Mg 2 0.471(5) 0.3984(5) 0.25 0.2492(1) 0.0153(6) Li2 Li 2 0.529(5) 0.3984(5) 0.25 0.2492(1) 0.0153(6) Mg3 Mg 2 0.210(4) 0.7433(7) 0.25 0.8013(2) 0.0123(9) Li3 Li 2 0.790(4) 0.7433(7) 0.25 0.8013(2) 0.0123(9) O1 O 1 1 0.5578(4) 0.1130(2) 0.8729(1) 0.0120(5) O2 O 2 1 0.1445(5) 0.25 0.1534(1) 0.0108(6) O3 O 1 1 0.4175(4) 0.1159(2) 0.0364(1) 0.0105(5) O4 O 2 1 0.9428(5) 0.25 0.9948(1) 0.0109(7) O5 O 1 1 0.3510(4) 0.8836(2) 0.7950(1) 0.0106(4) O6 O 1 1 0.0813(4) 0.9905(2) 0.9247(1) 0.0116(5) O7 O 1 1 0.0772(4) 0.1242(2) 0.7868(1) 0.0145(5) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo1 0.0080(1) 0.0071(1) 0.0065(1) 0 0.0001(1) 0 Mo2 0.00933(9) 0.00716(8) 0.00785(8) 0.00082(9) 0.00038(9) -0.00100(7) O1 0.0134(9) 0.0113(9) 0.0113(8) -0.0021(8) -0.0001(7) 0.0006(8) O2 0.014(1) 0.013(1) 0.006(1) 0 0.002(1) 0 O3 0.0102(8) 0.0094(8) 0.0119(8) 0.0010(7) 0.0010(7) -0.0021(7) O4 0.011(1) 0.010(1) 0.011(1) 0 0.000(1) 0 O5 0.0113(8) 0.0096(8) 0.0110(7) 0.0004(8) 0.0015(7) -0.0026(7) O6 0.0108(9) 0.0139(9) 0.0101(8) 0.0004(8) 0.0020(7) 0.0009(7) O7 0.0145(9) 0.0148(9) 0.0143(9) 0.0024(8) -0.0004(8) 0.0038(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mo1 O2 1.745(2) . . Mo1 O3 1.765(2) . . Mo1 O3 1.765(2) . 8_555 Mo1 O4 1.793(3) . 1_454 Mo2 O1 1.780(2) . . Mo2 O5 1.768(2) . 1_545 Mo2 O6 1.786(2) . 1_545 Mo2 O7 1.749(2) . . Mg1 O1 2.055(2) . . Mg1 O3 2.099(2) . 1_556 Mg1 O3 2.185(2) . 5_656 Mg1 O4 2.111(2) . . Mg1 O6 2.076(2) . 1_645 Mg1 O6 2.117(2) . 5_667 Mg2 O2 2.129(4) . . Mg2 O2 2.129(4) . 2_555 Mg2 O5 2.050(3) . 5_666 Mg2 O5 2.057(3) . 6_564 Mg2 O5 2.057(3) . 3_544 Mg2 O5 2.050(3) . 4_646 Mg3 O1 2.133(3) . . Mg3 O1 2.133(3) . 8_555 Mg3 O7 2.172(4) . 1_655 Mg3 O7 2.206(3) . 2_556 Mg3 O7 2.206(3) . 7_556 Mg3 O7 2.172(4) . 8_655 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_2 _geom_angle_site_symmetry_3 O2 Mo1 O3 109.03(8) . . . O2 Mo1 O3 109.03(8) . . 8_555 O2 Mo1 O4 114.7(1) . . 1_454 O3 Mo1 O3 105.30(9) . . 8_555 O3 Mo1 O4 109.16(8) . . 1_454 O3 Mo1 O3 105.30(9) 8_555 . . O3 Mo1 O4 109.16(8) 8_555 . 1_454 O1 Mo2 O5 113.16(8) . . 1_545 O1 Mo2 O6 108.97(9) . . 1_545 O1 Mo2 O7 110.02(9) . . . O5 Mo2 O6 109.16(8) 1_545 . 1_545 O5 Mo2 O7 110.21(8) 1_545 . . O6 Mo2 O7 104.99(9) 1_545 . . O1 Mg1 O3 91.29(9) . . 1_556 O1 Mg1 O3 85.56(8) . . 5_656 O1 Mg1 O4 102.5(1) . . . O1 Mg1 O6 97.55(9) . . 1_645 O1 Mg1 O6 171.1(1) . . 5_667 O3 Mg1 O3 84.14(8) 1_556 . 5_656 O3 Mg1 O4 95.6(1) 1_556 . . O3 Mg1 O6 165.0(1) 1_556 . 1_645 O3 Mg1 O6 86.11(8) 1_556 . 5_667 O3 Mg1 O3 84.14(8) 5_656 . 1_556 O3 Mg1 O4 171.9(1) 5_656 . . O3 Mg1 O6 84.53(8) 5_656 . 1_645 O3 Mg1 O6 85.67(8) 5_656 . 5_667 O4 Mg1 O6 94.2(1) . . 1_645 O4 Mg1 O6 86.3(1) . . 5_667 O6 Mg1 O6 83.32(9) 1_645 . 5_667 O6 Mg1 O6 83.32(9) 5_667 . 1_645 O2 Mg2 O2 178.7(2) . . 2_555 O2 Mg2 O5 94.7(1) . . 5_666 O2 Mg2 O5 86.1(1) . . 6_564 O2 Mg2 O5 86.1(1) . . 3_544 O2 Mg2 O5 94.7(1) . . 4_646 O2 Mg2 O2 178.7(2) 2_555 . . O2 Mg2 O5 86.3(1) 2_555 . 5_666 O2 Mg2 O5 92.9(1) 2_555 . 6_564 O2 Mg2 O5 92.9(1) 2_555 . 3_544 O2 Mg2 O5 86.3(1) 2_555 . 4_646 O5 Mg2 O5 94.20(7) 5_666 . 6_564 O5 Mg2 O5 179.2(2) 5_666 . 3_544 O5 Mg2 O5 86.0(1) 5_666 . 4_646 O5 Mg2 O5 94.20(7) 6_564 . 5_666 O5 Mg2 O5 85.6(1) 6_564 . 3_544 O5 Mg2 O5 179.2(2) 6_564 . 4_646 O5 Mg2 O5 179.2(2) 3_544 . 5_666 O5 Mg2 O5 85.6(1) 3_544 . 6_564 O5 Mg2 O5 94.20(7) 3_544 . 4_646 O5 Mg2 O5 86.0(1) 4_646 . 5_666 O5 Mg2 O5 179.2(2) 4_646 . 6_564 O5 Mg2 O5 94.20(7) 4_646 . 3_544 O1 Mg3 O1 84.5(1) . . 8_555 O1 Mg3 O7 90.68(9) . . 1_655 O1 Mg3 O7 81.0(1) . . 2_556 O1 Mg3 O7 130.3(2) . . 7_556 O1 Mg3 O7 145.8(2) . . 8_655 O1 Mg3 O1 84.5(1) 8_555 . . O1 Mg3 O7 145.8(2) 8_555 . 1_655 O1 Mg3 O7 130.3(2) 8_555 . 2_556 O1 Mg3 O7 81.0(1) 8_555 . 7_556 O1 Mg3 O7 90.68(9) 8_555 . 8_655 O7 Mg3 O7 81.9(1) 1_655 . 2_556 O7 Mg3 O7 125.6(2) 1_655 . 7_556 O7 Mg3 O7 74.6(1) 1_655 . 8_655 O7 Mg3 O7 81.9(1) 2_556 . 1_655 O7 Mg3 O7 73.3(1) 2_556 . 7_556 O7 Mg3 O7 125.6(2) 2_556 . 8_655 O7 Mg3 O7 125.6(2) 7_556 . 1_655 O7 Mg3 O7 73.3(1) 7_556 . 2_556 O7 Mg3 O7 81.9(1) 7_556 . 8_655 O7 Mg3 O7 74.6(1) 8_655 . 1_655 O7 Mg3 O7 125.6(2) 8_655 . 2_556 O7 Mg3 O7 81.9(1) 8_655 . 7_556