# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Ok, Kang Min' _publ_contact_author_address ; Department of Chemistry Chung-Ang University Seoul 156-756 Korea ; _publ_contact_author_email kmok@cau.ac.kr _publ_contact_author_fax 82(2)8254736 _publ_contact_author_phone 82(2)8205197 #------------------ TITLE AND AUTHOR LIST------------------------------------# _publ_section_title ; PbMSeO6 (M = Mo and W): New quaternary mixed metal selenites with asymmetric cationic coordination environments ; _publ_author_address ; Department of Chemistry Chung-Ang University Seoul 156-756 Korea ; loop_ _publ_author_name 'Dong Woo Lee' 'Kang Min Ok Seung-Jin Oh' data_SJ4 _database_code_depnum_ccdc_archive 'CCDC 849735' #TrackingRef '- PbSeMoO6.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'Mo2 O12 Pb2 Se2' _chemical_formula_weight 956.20 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _cell_length_a 6.8944(6) _cell_length_b 7.2219(6) _cell_length_c 10.8294(9) _cell_angle_alpha 99.751(2) _cell_angle_beta 99.996(2) _cell_angle_gamma 90.041(2) _cell_volume 523.09(8) _cell_formula_units_Z 2 _cell_measurement_temperature 200.0(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 6.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824.0 _exptl_crystal_description Needle _exptl_crystal_colour 'Light Yellow' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 41.450 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_process_details ; SADABS(Blessing, 1995) ; _exptl_absorpt_correction_T_min 0.39 _exptl_absorpt_correction_T_max 0.66 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'Bruker SMART Breeze' _diffrn_measurement_method CCD _diffrn_ambient_temperature 200.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_unetI/netI 0.0955 _diffrn_reflns_number 5065 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.35 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 2598 _reflns_number_gt 1896 _reflns_threshold_expression >2\(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0015(3) _refine_ls_number_reflns 2598 _refine_ls_number_parameters 104 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.126 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.526 _refine_diff_density_min -3.388 _refine_diff_density_rms 0.583 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pb1 Pb 0.24408(10) 0.13656(9) 0.49459(6) 0.0141(2) Uani 1 1 d . . . Pb2 Pb 0.35888(10) 0.29111(9) 0.15782(6) 0.0129(2) Uani 1 1 d . . . Mo1 Mo 0.8428(2) 0.04831(19) 0.19861(13) 0.0085(3) Uani 1 1 d . . . Mo2 Mo 0.8425(2) 0.5503(2) 0.20270(14) 0.0097(3) Uani 1 1 d . . . Se1 Se 0.7110(2) 0.3610(2) 0.46809(15) 0.0095(3) Uani 1 1 d . . . Se2 Se 0.3892(2) 0.8066(2) 0.21365(16) 0.0103(3) Uani 1 1 d . . . O1 O 0.831(2) -0.0460(19) 0.0430(13) 0.024(3) Uiso 1 1 d . . . O2 O 1.0936(19) 0.1077(18) 0.2420(12) 0.019(3) Uiso 1 1 d . . . O3 O 0.8671(17) -0.1714(16) 0.2742(11) 0.012(2) Uiso 1 1 d . . . O4 O 0.7375(16) 0.2895(15) 0.1751(10) 0.009(2) Uiso 1 1 d . . . O5 O 0.8148(17) 0.1531(16) 0.4011(11) 0.012(2) Uiso 1 1 d . . . O6 O 0.5210(19) 0.9703(17) 0.1736(12) 0.017(3) Uiso 1 1 d . . . O7 O 0.819(2) 0.5699(18) 0.0459(13) 0.023(3) Uiso 1 1 d . . . O8 O 1.0843(19) 0.4945(18) 0.2426(12) 0.021(3) Uiso 1 1 d . . . O9 O 0.7956(15) 0.5314(14) 0.3965(10) 0.006(2) Uiso 1 1 d . . . O10 O 0.520(2) 0.6049(18) 0.1849(13) 0.023(3) Uiso 1 1 d . . . O11 O 0.4743(17) 0.3313(16) 0.3929(11) 0.012(2) Uiso 1 1 d . . . O12 O 0.434(2) 0.8560(18) 0.3755(12) 0.023(3) Uiso 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 Pb1 0.0116(4) 0.0139(4) 0.0164(4) 0.0016(3) 0.0022(3) 0.0008(3) Pb2 0.0107(4) 0.0120(4) 0.0159(4) 0.0028(2) 0.0017(2) 0.0006(2) Mo1 0.0085(7) 0.0049(6) 0.0125(7) 0.0016(5) 0.0028(5) -0.0006(5) Mo2 0.0066(7) 0.0114(7) 0.0110(7) 0.0015(5) 0.0017(5) 0.0013(5) Se1 0.0098(8) 0.0063(8) 0.0133(8) 0.0026(6) 0.0036(6) 0.0002(6) Se2 0.0062(8) 0.0082(8) 0.0170(9) 0.0025(6) 0.0026(6) 0.0004(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Pb1 O12 2.410(14) 2_666 ? Pb1 O9 2.524(10) 2_666 ? Pb1 O5 2.603(11) 2_656 ? Pb1 O11 2.615(11) . ? Pb1 O12 2.679(13) 1_545 ? Pb1 O3 2.716(11) 2_656 ? Pb1 O2 2.724(13) 1_455 ? Pb1 O5 2.966(13) 1_455 ? Pb2 O10 2.473(13) . ? Pb2 O11 2.499(11) . ? Pb2 O4 2.584(11) . ? Pb2 O6 2.592(12) 1_545 ? Pb2 O8 2.596(13) 1_455 ? Pb2 O2 2.630(12) 1_455 ? Pb2 O7 2.683(13) 2_665 ? Pb2 O1 2.699(14) 2_655 ? Mo1 O1 1.696(13) . ? Mo1 O2 1.745(13) . ? Mo1 O3 1.899(11) . ? Mo1 O4 1.927(11) . ? Mo1 O5 2.237(11) . ? Mo1 O6 2.247(13) 1_545 ? Mo2 O7 1.708(13) . ? Mo2 O8 1.714(13) . ? Mo2 O4 1.973(11) . ? Mo2 O3 2.024(11) 1_565 ? Mo2 O9 2.204(10) . ? Mo2 O10 2.239(14) . ? Se1 O11 1.688(11) . ? Se1 O9 1.713(10) . ? Se1 O5 1.762(12) . ? Se2 O6 1.649(12) . ? Se2 O12 1.701(13) . ? Se2 O10 1.725(14) . ? O1 Pb2 2.699(14) 2_655 ? O2 Pb2 2.630(12) 1_655 ? O2 Pb1 2.724(13) 1_655 ? O3 Mo2 2.024(11) 1_545 ? O3 Pb1 2.716(11) 2_656 ? O5 Pb1 2.603(11) 2_656 ? O6 Mo1 2.247(13) 1_565 ? O6 Pb2 2.592(12) 1_565 ? O7 Pb2 2.683(13) 2_665 ? O8 Pb2 2.596(13) 1_655 ? O9 Pb1 2.524(10) 2_666 ? O12 Pb1 2.410(14) 2_666 ? O12 Pb1 2.679(13) 1_565 ? 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 O12 Pb1 O9 88.1(4) 2_666 2_666 ? O12 Pb1 O5 83.3(4) 2_666 2_656 ? O9 Pb1 O5 121.9(3) 2_666 2_656 ? O12 Pb1 O11 73.7(4) 2_666 . ? O9 Pb1 O11 77.5(3) 2_666 . ? O5 Pb1 O11 149.7(4) 2_656 . ? O12 Pb1 O12 75.1(5) 2_666 1_545 ? O9 Pb1 O12 155.2(4) 2_666 1_545 ? O5 Pb1 O12 74.7(4) 2_656 1_545 ? O11 Pb1 O12 80.3(4) . 1_545 ? O12 Pb1 O3 81.5(4) 2_666 2_656 ? O9 Pb1 O3 64.3(3) 2_666 2_656 ? O5 Pb1 O3 57.7(3) 2_656 2_656 ? O11 Pb1 O3 134.8(3) . 2_656 ? O12 Pb1 O3 128.9(4) 1_545 2_656 ? O12 Pb1 O2 136.7(4) 2_666 1_455 ? O9 Pb1 O2 108.7(3) 2_666 1_455 ? O5 Pb1 O2 116.4(4) 2_656 1_455 ? O11 Pb1 O2 71.7(4) . 1_455 ? O12 Pb1 O2 74.1(4) 1_545 1_455 ? O3 Pb1 O2 141.8(4) 2_656 1_455 ? O10 Pb2 O11 82.9(4) . . ? O10 Pb2 O4 65.2(4) . . ? O11 Pb2 O4 77.8(3) . . ? O10 Pb2 O6 128.6(4) . 1_545 ? O11 Pb2 O6 80.0(4) . 1_545 ? O4 Pb2 O6 64.0(4) . 1_545 ? O10 Pb2 O8 81.1(4) . 1_455 ? O11 Pb2 O8 78.5(4) . 1_455 ? O4 Pb2 O8 140.7(4) . 1_455 ? O6 Pb2 O8 140.2(4) 1_545 1_455 ? O10 Pb2 O2 142.1(4) . 1_455 ? O11 Pb2 O2 75.1(4) . 1_455 ? O4 Pb2 O2 136.1(4) . 1_455 ? O6 Pb2 O2 77.7(4) 1_545 1_455 ? O8 Pb2 O2 64.6(4) 1_455 1_455 ? O10 Pb2 O7 76.5(4) . 2_665 ? O11 Pb2 O7 149.6(4) . 2_665 ? O4 Pb2 O7 112.3(4) . 2_665 ? O6 Pb2 O7 130.4(4) 1_545 2_665 ? O8 Pb2 O7 76.4(4) 1_455 2_665 ? O2 Pb2 O7 108.6(4) 1_455 2_665 ? O10 Pb2 O1 134.7(4) . 2_655 ? O11 Pb2 O1 142.4(4) . 2_655 ? O4 Pb2 O1 113.0(4) . 2_655 ? O6 Pb2 O1 74.0(4) 1_545 2_655 ? O8 Pb2 O1 105.0(4) 1_455 2_655 ? O2 Pb2 O1 73.1(4) 1_455 2_655 ? O7 Pb2 O1 62.2(4) 2_665 2_655 ? O1 Mo1 O2 100.4(6) . . ? O1 Mo1 O3 100.9(6) . . ? O2 Mo1 O3 93.4(5) . . ? O1 Mo1 O4 97.9(5) . . ? O2 Mo1 O4 100.5(5) . . ? O3 Mo1 O4 154.2(5) . . ? O1 Mo1 O5 171.7(6) . . ? O2 Mo1 O5 87.7(5) . . ? O3 Mo1 O5 76.3(4) . . ? O4 Mo1 O5 82.6(4) . . ? O1 Mo1 O6 87.4(6) . 1_545 ? O2 Mo1 O6 171.4(5) . 1_545 ? O3 Mo1 O6 81.6(5) . 1_545 ? O4 Mo1 O6 81.7(4) . 1_545 ? O5 Mo1 O6 84.4(4) . 1_545 ? O7 Mo2 O8 103.4(6) . . ? O7 Mo2 O4 96.8(5) . . ? O8 Mo2 O4 95.4(5) . . ? O7 Mo2 O3 97.1(5) . 1_565 ? O8 Mo2 O3 98.7(6) . 1_565 ? O4 Mo2 O3 157.3(5) . 1_565 ? O7 Mo2 O9 166.4(5) . . ? O8 Mo2 O9 90.1(5) . . ? O4 Mo2 O9 79.8(4) . . ? O3 Mo2 O9 82.5(4) 1_565 . ? O7 Mo2 O10 87.1(6) . . ? O8 Mo2 O10 169.1(5) . . ? O4 Mo2 O10 80.4(5) . . ? O3 Mo2 O10 82.5(5) 1_565 . ? O9 Mo2 O10 79.3(4) . . ? O11 Se1 O9 101.6(5) . . ? O11 Se1 O5 101.5(6) . . ? O9 Se1 O5 104.3(5) . . ? O6 Se2 O12 103.2(6) . . ? O6 Se2 O10 104.1(6) . . ? O12 Se2 O10 101.7(6) . . ? Mo1 O1 Pb2 146.3(7) . 2_655 ? Mo1 O2 Pb2 137.5(6) . 1_655 ? Mo1 O2 Pb1 115.5(6) . 1_655 ? Pb2 O2 Pb1 103.0(4) 1_655 1_655 ? Mo1 O3 Mo2 133.5(6) . 1_545 ? Mo1 O3 Pb1 115.2(5) . 2_656 ? Mo2 O3 Pb1 105.4(4) 1_545 2_656 ? Mo1 O4 Mo2 136.1(6) . . ? Mo1 O4 Pb2 112.2(5) . . ? Mo2 O4 Pb2 109.5(5) . . ? Se1 O5 Mo1 129.6(6) . . ? Se1 O5 Pb1 114.1(5) . 2_656 ? Mo1 O5 Pb1 108.0(4) . 2_656 ? Se2 O6 Mo1 136.2(7) . 1_565 ? Se2 O6 Pb2 117.1(6) . 1_565 ? Mo1 O6 Pb2 101.8(4) 1_565 1_565 ? Mo2 O7 Pb2 150.9(7) . 2_665 ? Mo2 O8 Pb2 142.3(7) . 1_655 ? Se1 O9 Mo2 135.5(6) . . ? Se1 O9 Pb1 114.4(5) . 2_666 ? Mo2 O9 Pb1 106.5(4) . 2_666 ? Se2 O10 Mo2 133.1(7) . . ? Se2 O10 Pb2 120.8(7) . . ? Mo2 O10 Pb2 104.9(5) . . ? Se1 O11 Pb2 125.8(6) . . ? Se1 O11 Pb1 115.9(5) . . ? Pb2 O11 Pb1 110.0(4) . . ? Se2 O12 Pb1 124.3(7) . 2_666 ? Se2 O12 Pb1 119.3(6) . 1_565 ? Pb1 O12 Pb1 104.9(5) 2_666 1_565 ? #===END