# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics # This journal is © The Owner Societies 2012 data_publication_text _journal_name_full Phys.Chem.Chem.Phys.(PCCP) _journal_coden_cambridge 1326 #TrackingRef 'Data for 1.cif' _publ_contact_author_name 'Pratim Chattaraj' _publ_contact_author_address ;Department of Chemistry Indian Institute of Technology Kharagpur 721302 India ; _publ_contact_author_email pratim.chattaraj@gmail.com loop_ _publ_author_name _publ_author_address 'Pratim Chattaraj' ;Department of Chemistry Indian Institute of Technology Kharagpur 721302 India ; 'Dibakar Deb' '' 'Soma Duley' '' 'Slavko Radenkovic' '' 'Patrick Bultinck' '' 'Manish Bhattacharjee' '' #============================================================================== #============================================================================== #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_struct _database_code_depnum_ccdc_archive 'CCDC 902736' #TrackingRef 'Data for 1.cif' _audit_creation_date 2011-08-30T14:32:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C6 H10 K1 Li2 Mo1 N1 O11' _chemical_formula_sum 'C6 H10 K1 Li2 Mo1 N1 O11' _chemical_formula_weight 421.07 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.9807(10) _cell_length_b 8.5886(11) _cell_length_c 20.424(3) _cell_angle_alpha 90 _cell_angle_beta 96.724(4) _cell_angle_gamma 90 _cell_volume 1390.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.297 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_unetI/netI 0.0491 _diffrn_reflns_number 17378 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.46 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 2837 _reflns_number_gt 2226 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^)+(0.0264P)^2^+1.1974P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment refall _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 0.0011(3) _refine_ls_number_reflns 2837 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.071 _refine_ls_wR_factor_gt 0.066 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.494 _refine_diff_density_min -0.5 _refine_diff_density_rms 0.109 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_number_in_cell C 24 H 40 K 4 Li 8 Mo 4 N 4 O 44 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 C1 C 0.1137(5) 0.6393(5) 0.34178(18) 0.0268(10) Uani 1 1 d . . . H1A H 0.0547 0.551 0.3203 0.032 Uiso 1 1 calc R . . H1B H 0.0322 0.7225 0.3437 0.032 Uiso 1 1 calc R . . C2 C 0.1801(5) 0.5934(4) 0.41108(17) 0.0194(8) Uani 1 1 d . . . C3 C 0.2582(5) 0.8620(4) 0.2992(2) 0.0302(10) Uani 1 1 d . . . H3A H 0.1485 0.907 0.3034 0.036 Uiso 1 1 calc R . . H3B H 0.2892 0.8923 0.2564 0.036 Uiso 1 1 calc R . . C4 C 0.3848(5) 0.9295(4) 0.35190(18) 0.0177(8) Uani 1 1 d . . . C5 C 0.2108(5) 0.6299(4) 0.23273(17) 0.0213(9) Uani 1 1 d . . . H5A H 0.2109 0.5171 0.2351 0.026 Uiso 1 1 calc R . . H5B H 0.3041 0.6603 0.2091 0.026 Uiso 1 1 calc R . . C6 C 0.0461(5) 0.6813(4) 0.19185(19) 0.0223(9) Uani 1 1 d . . . Li1 Li 0.8607(8) 0.5923(8) 0.4788(3) 0.0272(15) Uani 1 1 d . . . Li2 Li -0.3067(8) 0.7324(7) 0.2043(3) 0.0205(14) Uani 1 1 d . . . O1W O -0.1795(4) 0.7213(4) 0.02653(18) 0.0354(8) Uani 1 1 d . . . O2W O 0.2565(5) 0.5322(5) 0.05307(18) 0.0413(9) Uani 1 1 d . . . O5 O 0.0791(3) 0.5694(3) 0.45174(13) 0.0309(7) Uani 1 1 d . . . O7 O 0.3906(3) 1.0711(3) 0.35969(13) 0.0262(6) Uani 1 1 d . . . O8 O 0.0351(4) 0.6401(4) 0.13291(14) 0.0497(9) Uani 1 1 d . . . O9 O -0.0631(3) 0.7525(3) 0.21818(13) 0.0244(6) Uani 1 1 d . . . H1W" H -0.183(7) 0.640(7) 0.007(3) 0.07(2) Uiso 1 1 d . . . H1W' H -0.128(6) 0.702(5) 0.061(2) 0.036(15) Uiso 1 1 d . . . H2W' H 0.324(8) 0.483(7) 0.072(3) 0.07(2) Uiso 1 1 d . . . H2W" H 0.178(8) 0.580(7) 0.074(3) 0.10(2) Uiso 1 1 d . . . N1 N 0.2437(4) 0.6914(3) 0.30105(14) 0.0139(6) Uani 1 1 d . . . O1 O 0.6086(3) 0.6670(3) 0.28555(13) 0.0269(7) Uani 1 1 d . . . O2 O 0.6700(3) 0.5620(3) 0.41528(12) 0.0237(6) Uani 1 1 d . . . O3 O 0.4421(3) 0.4114(3) 0.32478(13) 0.0259(6) Uani 1 1 d . . . O4 O 0.3364(3) 0.5757(3) 0.42511(12) 0.0257(6) Uani 1 1 d . . . O6 O 0.4829(3) 0.8334(3) 0.38512(13) 0.0271(7) Uani 1 1 d . . . K1 K 0.51831(12) 0.27403(10) 0.46170(5) 0.0333(2) Uani 1 1 d . . . Mo1 Mo 0.51262(4) 0.59539(3) 0.350305(15) 0.01325(11) 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 C1 0.015(2) 0.049(3) 0.017(2) 0.0123(18) 0.0015(16) -0.0009(18) C2 0.020(2) 0.0222(18) 0.0164(19) 0.0000(16) 0.0028(15) 0.0007(17) C3 0.036(3) 0.016(2) 0.034(2) 0.0035(17) -0.016(2) -0.0015(17) C4 0.0167(19) 0.0188(19) 0.0178(19) -0.0007(15) 0.0029(15) 0.0003(15) C5 0.019(2) 0.030(2) 0.0136(19) -0.0029(16) -0.0044(16) 0.0017(16) C6 0.019(2) 0.028(2) 0.018(2) 0.0027(16) -0.0038(17) -0.0040(17) Li1 0.021(4) 0.038(4) 0.022(4) 0.004(3) 0.003(3) 0.003(3) Li2 0.020(3) 0.021(3) 0.020(3) 0.004(3) 0.000(3) 0.001(3) O1W 0.039(2) 0.042(2) 0.0225(18) 0.0045(16) -0.0074(16) 0.0021(16) O2W 0.030(2) 0.051(2) 0.041(2) -0.0046(17) -0.0021(17) 0.0083(17) O5 0.0195(15) 0.054(2) 0.0213(15) 0.0142(13) 0.0102(12) 0.0043(13) O7 0.0344(16) 0.0160(14) 0.0260(15) -0.0017(11) -0.0060(12) 0.0012(12) O8 0.0388(19) 0.090(3) 0.0171(16) -0.0140(16) -0.0097(14) 0.0268(18) O9 0.0180(15) 0.0330(16) 0.0217(15) -0.0010(12) -0.0003(12) 0.0041(12) N1 0.0142(16) 0.0166(15) 0.0110(15) 0.0014(12) 0.0019(12) -0.0026(12) O1 0.0224(16) 0.0379(16) 0.0220(15) 0.0084(12) 0.0087(12) -0.0005(12) O2 0.0184(14) 0.0301(15) 0.0211(14) 0.0008(11) -0.0043(11) 0.0000(11) O3 0.0287(15) 0.0173(13) 0.0302(15) -0.0022(12) -0.0034(12) -0.0002(12) O4 0.0151(14) 0.0456(18) 0.0168(14) 0.0073(12) 0.0040(11) 0.0036(12) O6 0.0302(16) 0.0184(13) 0.0289(16) -0.0031(12) -0.0123(13) 0.0048(12) K1 0.0379(6) 0.0289(5) 0.0306(5) -0.0013(4) -0.0058(4) -0.0009(4) Mo1 0.01237(17) 0.01486(16) 0.01216(17) 0.00045(13) -0.00007(11) -0.00003(14) #----------------------------------------------------------------------------# # 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 C1 N1 1.473(4) . ? C1 C2 1.504(5) . ? C2 O5 1.240(4) . ? C2 O4 1.257(4) . ? C2 K1 3.518(4) 3_666 ? C3 N1 1.471(4) . ? C3 C4 1.504(5) . ? C4 O7 1.227(4) . ? C4 O6 1.277(4) . ? C5 N1 1.486(4) . ? C5 C6 1.537(5) . ? C6 O9 1.238(4) . ? C6 O8 1.248(5) . ? Li1 O2 1.898(7) . ? Li1 O5 1.899(7) 1_655 ? Li1 O1W 1.921(8) 4_676 ? Li1 O5 2.004(7) 3_666 ? Li1 Li1 2.786(13) 3_766 ? Li1 K1 3.579(7) 3_666 ? Li1 K1 3.852(7) . ? Li2 O3 1.932(7) 2 ? Li2 O9 1.939(7) . ? Li2 O1 1.946(7) 1_455 ? Li2 O7 1.967(7) 2_545 ? Li2 K1 3.624(6) 2 ? O1W Li1 1.921(8) 4_475 ? O1W K1 2.780(4) 2 ? O2W K1 2.785(4) 2_655 ? O5 Li1 1.899(7) 1_455 ? O5 Li1 2.004(7) 3_666 ? O7 Li2 1.967(7) 2 ? O7 K1 2.814(3) 1_565 ? N1 Mo1 2.407(3) . ? O1 Mo1 1.718(2) . ? O1 Li2 1.946(7) 1_655 ? O2 Mo1 1.741(2) . ? O2 K1 2.958(3) . ? O2 K1 3.382(3) 3_666 ? O3 Mo1 1.737(2) . ? O3 Li2 1.932(7) 2_545 ? O3 K1 3.030(3) . ? O4 Mo1 2.201(2) . ? O4 K1 2.780(3) 3_666 ? O4 K1 3.021(3) . ? O6 Mo1 2.186(3) . ? O6 K1 3.263(3) 3_666 ? K1 O4 2.780(3) 3_666 ? K1 O1W 2.780(4) 2_545 ? K1 O2W 2.786(4) 2_645 ? K1 O7 2.814(3) 1_545 ? K1 O6 3.263(3) 3_666 ? K1 O2 3.382(3) 3_666 ? K1 C2 3.518(4) 3_666 ? K1 Mo1 3.5737(10) . ? K1 Li1 3.579(7) 3_666 ? Mo1 K1 4.0353(11) 3_666 ? 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 N1 C1 C2 114.7(3) . . ? O5 C2 O4 122.2(3) . . ? O5 C2 C1 119.3(3) . . ? O4 C2 C1 118.5(3) . . ? O5 C2 K1 90.1(2) . 3_666 ? O4 C2 K1 45.20(18) . 3_666 ? C1 C2 K1 138.2(2) . 3_666 ? N1 C3 C4 114.4(3) . . ? O7 C4 O6 124.1(3) . . ? O7 C4 C3 119.1(3) . . ? O6 C4 C3 116.8(3) . . ? N1 C5 C6 117.0(3) . . ? O9 C6 O8 125.9(4) . . ? O9 C6 C5 120.4(3) . . ? O8 C6 C5 113.7(3) . . ? O2 Li1 O5 118.5(4) . 1_655 ? O2 Li1 O1W 107.0(3) . 4_676 ? O5 Li1 O1W 116.6(4) 1_655 4_676 ? O2 Li1 O5 119.7(4) . 3_666 ? O5 Li1 O5 89.0(3) 1_655 3_666 ? O1W Li1 O5 105.0(3) 4_676 3_666 ? O2 Li1 Li1 132.9(5) . 3_766 ? O5 Li1 Li1 46.0(2) 1_655 3_766 ? O1W Li1 Li1 119.4(4) 4_676 3_766 ? O5 Li1 Li1 43.0(2) 3_666 3_766 ? O2 Li1 K1 68.5(2) . 3_666 ? O5 Li1 K1 166.7(3) 1_655 3_666 ? O1W Li1 K1 50.37(18) 4_676 3_666 ? O5 Li1 K1 97.1(2) 3_666 3_666 ? Li1 Li1 K1 138.8(3) 3_766 3_666 ? O2 Li1 K1 48.49(18) . . ? O5 Li1 K1 124.4(3) 1_655 . ? O1W Li1 K1 118.6(3) 4_676 . ? O5 Li1 K1 71.4(2) 3_666 . ? Li1 Li1 K1 99.0(3) 3_766 . ? K1 Li1 K1 68.87(12) 3_666 . ? O3 Li2 O9 119.3(3) 2 . ? O3 Li2 O1 104.7(3) 2 1_455 ? O9 Li2 O1 110.1(3) . 1_455 ? O3 Li2 O7 102.8(3) 2 2_545 ? O9 Li2 O7 114.7(3) . 2_545 ? O1 Li2 O7 103.8(3) 1_455 2_545 ? O3 Li2 K1 56.72(17) 2 2 ? O9 Li2 K1 118.5(3) . 2 ? O1 Li2 K1 131.0(3) 1_455 2 ? O7 Li2 K1 50.42(16) 2_545 2 ? Li1 O1W K1 97.5(2) 4_475 2 ? C2 O5 Li1 150.2(3) . 1_455 ? C2 O5 Li1 118.0(3) . 3_666 ? Li1 O5 Li1 91.0(3) 1_455 3_666 ? C4 O7 Li2 127.4(3) . 2 ? C4 O7 K1 135.6(2) . 1_565 ? Li2 O7 K1 97.0(2) 2 1_565 ? C6 O9 Li2 129.6(3) . . ? C3 N1 C1 112.4(3) . . ? C3 N1 C5 109.6(3) . . ? C1 N1 C5 111.3(3) . . ? C3 N1 Mo1 106.5(2) . . ? C1 N1 Mo1 108.2(2) . . ? C5 N1 Mo1 108.7(2) . . ? Mo1 O1 Li2 172.0(2) . 1_655 ? Mo1 O2 Li1 161.3(3) . . ? Mo1 O2 K1 95.52(10) . . ? Li1 O2 K1 102.8(2) . . ? Mo1 O2 K1 98.86(10) . 3_666 ? Li1 O2 K1 80.0(2) . 3_666 ? K1 O2 K1 82.87(7) . 3_666 ? Mo1 O3 Li2 165.0(2) . 2_545 ? Mo1 O3 K1 93.11(10) . . ? Li2 O3 K1 91.1(2) 2_545 . ? C2 O4 Mo1 122.1(2) . . ? C2 O4 K1 116.1(2) . 3_666 ? Mo1 O4 K1 107.68(10) . 3_666 ? C2 O4 K1 126.6(2) . . ? Mo1 O4 K1 84.84(8) . . ? K1 O4 K1 92.92(7) 3_666 . ? C4 O6 Mo1 121.0(2) . . ? C4 O6 K1 128.4(2) . 3_666 ? Mo1 O6 K1 93.44(9) . 3_666 ? O4 K1 O1W 108.59(9) 3_666 2_545 ? O4 K1 O2W 102.99(10) 3_666 2_645 ? O1W K1 O2W 122.30(12) 2_545 2_645 ? O4 K1 O7 169.39(8) 3_666 1_545 ? O1W K1 O7 72.03(9) 2_545 1_545 ? O2W K1 O7 68.93(10) 2_645 1_545 ? O4 K1 O2 74.45(8) 3_666 . ? O1W K1 O2 127.06(10) 2_545 . ? O2W K1 O2 107.18(10) 2_645 . ? O7 K1 O2 114.01(8) 1_545 . ? O4 K1 O4 87.08(7) 3_666 . ? O1W K1 O4 73.56(9) 2_545 . ? O2W K1 O4 155.51(10) 2_645 . ? O7 K1 O4 103.07(8) 1_545 . ? O2 K1 O4 53.58(7) . . ? O4 K1 O3 127.29(8) 3_666 . ? O1W K1 O3 92.92(10) 2_545 . ? O2W K1 O3 104.64(9) 2_645 . ? O7 K1 O3 62.72(7) 1_545 . ? O2 K1 O3 54.85(7) . . ? O4 K1 O3 53.06(7) . . ? O4 K1 O6 51.80(7) 3_666 3_666 ? O1W K1 O6 76.04(10) 2_545 3_666 ? O2W K1 O6 88.13(9) 2_645 3_666 ? O7 K1 O6 119.55(7) 1_545 3_666 ? O2 K1 O6 126.23(7) . 3_666 ? O4 K1 O6 115.11(7) . 3_666 ? O3 K1 O6 166.42(8) . 3_666 ? O4 K1 O2 50.74(7) 3_666 3_666 ? O1W K1 O2 58.81(8) 2_545 3_666 ? O2W K1 O2 137.66(9) 2_645 3_666 ? O7 K1 O2 130.83(8) 1_545 3_666 ? O2 K1 O2 97.13(7) . 3_666 ? O4 K1 O2 65.43(7) . 3_666 ? O3 K1 O2 117.70(7) . 3_666 ? O6 K1 O2 49.75(6) 3_666 3_666 ? O4 K1 C2 18.71(8) 3_666 3_666 ? O1W K1 C2 125.25(10) 2_545 3_666 ? O2W K1 C2 85.81(10) 2_645 3_666 ? O7 K1 C2 154.74(9) 1_545 3_666 ? O2 K1 C2 72.29(8) . 3_666 ? O4 K1 C2 99.94(8) . 3_666 ? O3 K1 C2 126.99(8) . 3_666 ? O6 K1 C2 57.45(8) 3_666 3_666 ? O2 K1 C2 69.00(7) 3_666 3_666 ? O4 K1 Mo1 98.27(6) 3_666 . ? O1W K1 Mo1 103.94(9) 2_545 . ? O2W K1 Mo1 117.85(8) 2_645 . ? O7 K1 Mo1 91.75(6) 1_545 . ? O2 K1 Mo1 29.00(5) . . ? O4 K1 Mo1 37.82(5) . . ? O3 K1 Mo1 29.04(5) . . ? O6 K1 Mo1 145.85(5) 3_666 . ? O2 K1 Mo1 100.24(5) 3_666 . ? C2 K1 Mo1 100.19(6) 3_666 . ? O4 K1 Li1 81.68(12) 3_666 3_666 ? O1W K1 Li1 32.15(13) 2_545 3_666 ? O2W K1 Li1 149.04(14) 2_645 3_666 ? O7 K1 Li1 101.70(13) 1_545 3_666 ? O2 K1 Li1 103.57(12) . 3_666 ? O4 K1 Li1 53.71(12) . 3_666 ? O3 K1 Li1 95.87(12) . 3_666 ? O6 K1 Li1 70.57(12) 3_666 3_666 ? O2 K1 Li1 31.49(11) 3_666 3_666 ? C2 K1 Li1 100.24(12) 3_666 3_666 ? Mo1 K1 Li1 91.16(11) . 3_666 ? O1 Mo1 O3 104.63(13) . . ? O1 Mo1 O2 107.40(12) . . ? O3 Mo1 O2 104.99(12) . . ? O1 Mo1 O6 89.47(12) . . ? O3 Mo1 O6 154.77(11) . . ? O2 Mo1 O6 90.11(11) . . ? O1 Mo1 O4 160.17(11) . . ? O3 Mo1 O4 85.84(11) . . ? O2 Mo1 O4 85.45(11) . . ? O6 Mo1 O4 75.15(10) . . ? O1 Mo1 N1 90.67(11) . . ? O3 Mo1 N1 86.82(11) . . ? O2 Mo1 N1 154.62(11) . . ? O6 Mo1 N1 71.96(10) . . ? O4 Mo1 N1 72.87(9) . . ? O1 Mo1 K1 142.46(9) . . ? O3 Mo1 K1 57.86(9) . . ? O2 Mo1 K1 55.48(8) . . ? O6 Mo1 K1 120.59(7) . . ? O4 Mo1 K1 57.33(7) . . ? N1 Mo1 K1 118.36(7) . . ? O1 Mo1 K1 135.69(10) . 3_666 ? O3 Mo1 K1 118.99(9) . 3_666 ? O2 Mo1 K1 55.90(9) . 3_666 ? O6 Mo1 K1 53.82(7) . 3_666 ? O4 Mo1 K1 41.02(7) . 3_666 ? N1 Mo1 K1 98.72(7) . 3_666 ? K1 Mo1 K1 66.83(2) . 3_666 ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment 'Data for 2.cif' data_struct1 _database_code_depnum_ccdc_archive 'CCDC 902737' #TrackingRef 'Data for 2.cif' _audit_creation_date 2011-07-18T11:17:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C6 H10 Li2 Mo1 N1 O11 Rb1' _chemical_formula_sum 'C6 H10 Li2 Mo1 N1 O11 Rb1' _chemical_formula_weight 467.44 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.9395(4) _cell_length_b 8.6813(4) _cell_length_c 20.6799(10) _cell_angle_alpha 90 _cell_angle_beta 96.7070(13) _cell_angle_gamma 90 _cell_volume 1415.61(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.396 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_unetI/netI 0.0342 _diffrn_reflns_number 20070 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 31.18 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.902 _reflns_number_total 4578 _reflns_number_gt 3350 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^)+(0.0314P)^2^+0.9924P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment refall _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 0.0021(2) _refine_ls_number_reflns 4132 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0611 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.01 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.301 _refine_diff_density_min -0.839 _refine_diff_density_rms 0.108 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_number_in_cell C 24 H 40 Li 8 Mo 4 N 4 O 44 Rb 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 C4 C 0.1175(3) 0.0798(3) 0.15026(12) 0.0193(5) Uani 1 1 d . . . O1 O -0.1059(2) 0.3354(2) 0.21442(9) 0.0281(4) Uani 1 1 d . . . O2 O -0.1720(2) 0.4377(2) 0.08609(9) 0.0240(4) Uani 1 1 d . . . O1W O 0.6704(3) 0.2740(3) 0.47189(13) 0.0401(6) Uani 1 1 d . . . O3 O 0.0527(2) 0.59411(19) 0.17561(9) 0.0246(4) Uani 1 1 d . . . O2W O 0.2565(3) 0.4949(3) 0.44113(13) 0.0431(6) Uani 1 1 d . . . O4 O 0.1653(2) 0.4343(2) 0.07743(9) 0.0246(4) Uani 1 1 d . . . O5 O 0.4215(2) 0.4296(3) 0.04876(10) 0.0329(5) Uani 1 1 d . . . O6 O 0.0228(2) 0.17446(19) 0.11568(9) 0.0256(4) Uani 1 1 d . . . O7 O 0.1089(2) -0.0613(2) 0.14359(10) 0.0282(4) Uani 1 1 d . . . O8 O 0.4682(3) 0.3669(4) 0.36509(11) 0.0564(8) Uani 1 1 d . . . O9 O 0.5657(2) 0.2528(2) 0.28143(9) 0.0259(4) Uani 1 1 d . . . Li1 Li 0.6397(6) 0.4072(6) 0.0205(2) 0.0282(10) Uani 1 1 d . . . Li2 Li 0.8097(5) 0.2727(5) 0.2953(2) 0.0202(9) Uani 1 1 d . . . H1' H 0.463(6) 0.439(5) 0.179(2) 0.070(14) Uiso 1 1 d . . . H1 H 0.457(5) 0.279(5) 0.153(2) 0.059(12) Uiso 1 1 d . . . H2 H 0.335(5) 0.110(4) 0.2023(19) 0.053(12) Uiso 1 1 d . . . H2' H 0.190(6) 0.124(5) 0.245(2) 0.088(16) Uiso 1 1 d . . . H1W' H 0.677(5) 0.352(5) 0.491(2) 0.047(12) Uiso 1 1 d . . . H1W H 0.617(6) 0.301(5) 0.439(2) 0.072(15) Uiso 1 1 d . . . H3 H 0.203(4) 0.361(3) 0.2905(15) 0.024(8) Uiso 1 1 d . . . H3' H 0.298(4) 0.490(4) 0.2613(17) 0.048(10) Uiso 1 1 d . . . H2W' H 0.196(6) 0.549(5) 0.420(2) 0.065(15) Uiso 1 1 d . . . H2W H 0.323(7) 0.448(6) 0.416(3) 0.099(19) Uiso 1 1 d . . . Rb1 Rb -0.03312(4) 0.73753(3) 0.037537(14) 0.03454(9) Uani 1 1 d . . . Mo1 Mo -0.01185(2) 0.41004(2) 0.150320(9) 0.01324(7) Uani 1 1 d . . . C2 C 0.3220(3) 0.4108(3) 0.08996(12) 0.0192(5) Uani 1 1 d . . . N1 N 0.2587(2) 0.3158(2) 0.19909(9) 0.0142(4) Uani 1 1 d . . . C5 C 0.2937(3) 0.3799(3) 0.26584(13) 0.0229(5) Uani 1 1 d . . . C6 C 0.4563(3) 0.3253(3) 0.30696(13) 0.0228(5) Uani 1 1 d . . . C1 C 0.3908(3) 0.3630(4) 0.15805(15) 0.0320(7) Uani 1 1 d . . . C3 C 0.2416(4) 0.1471(3) 0.20318(16) 0.0295(7) 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 C4 0.0196(11) 0.0186(11) 0.0195(12) 0.0004(9) 0.0013(10) -0.0014(9) O1 0.0248(10) 0.0368(11) 0.0240(10) 0.0079(8) 0.0086(8) -0.0019(8) O2 0.0201(9) 0.0284(9) 0.0219(9) 0.0019(8) -0.0045(7) 0.0004(7) O1W 0.0496(15) 0.0384(13) 0.0290(13) 0.0030(11) -0.0089(11) 0.0071(11) O3 0.0272(9) 0.0175(8) 0.0276(10) -0.0043(7) -0.0036(8) -0.0018(7) O2W 0.0365(13) 0.0514(15) 0.0390(14) -0.0047(12) -0.0058(11) 0.0101(11) O4 0.0165(8) 0.0403(11) 0.0172(9) 0.0070(8) 0.0024(7) 0.0025(8) O5 0.0203(9) 0.0567(13) 0.0234(10) 0.0167(10) 0.0099(8) 0.0037(9) O6 0.0296(10) 0.0165(8) 0.0273(10) -0.0035(7) -0.0108(8) 0.0019(7) O7 0.0369(11) 0.0159(8) 0.0295(10) -0.0010(7) -0.0063(9) 0.0005(7) O8 0.0467(14) 0.098(2) 0.0209(11) -0.0162(12) -0.0116(10) 0.0363(14) O9 0.0159(9) 0.0330(10) 0.0279(11) -0.0008(8) -0.0017(8) 0.0025(7) Li1 0.017(2) 0.043(3) 0.024(2) 0.002(2) 0.0000(18) -0.0002(19) Li2 0.020(2) 0.0197(19) 0.020(2) 0.0022(16) 0.0007(17) -0.0011(16) Rb1 0.04585(19) 0.02701(14) 0.02804(16) -0.00055(11) -0.00719(13) -0.00266(12) Mo1 0.01181(10) 0.01460(10) 0.01300(11) 0.00066(7) 0.00009(7) -0.00030(7) C2 0.0182(11) 0.0238(11) 0.0158(12) 0.0009(10) 0.0033(10) -0.0010(10) N1 0.0146(9) 0.0156(9) 0.0124(10) 0.0014(7) 0.0008(8) -0.0012(7) C5 0.0206(13) 0.0300(14) 0.0165(12) -0.0037(10) -0.0050(11) 0.0062(10) C6 0.0216(12) 0.0274(13) 0.0182(13) -0.0004(10) -0.0019(10) 0.0022(10) C1 0.0144(12) 0.060(2) 0.0222(15) 0.0147(14) 0.0030(11) 0.0007(13) C3 0.0335(16) 0.0163(11) 0.0343(17) -0.0001(11) -0.0146(14) 0.0005(11) #----------------------------------------------------------------------------# # 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 C4 O7 1.234(3) . ? C4 O6 1.275(3) . ? C4 C3 1.502(4) . ? O1 Mo1 1.7223(18) . ? O1 Li2 1.951(5) 1_455 ? O2 Mo1 1.7447(17) . ? O2 Li1 1.916(5) 1_455 ? O2 Rb1 3.0423(18) . ? O2 Rb1 3.5321(19) 3_565 ? O1W Li1 1.898(6) 4_566 ? O1W Rb1 2.926(3) 2_645 ? O3 Mo1 1.7399(17) . ? O3 Li2 1.951(4) 2_655 ? O3 Rb1 3.1166(19) . ? O2W Rb1 2.918(3) 2_545 ? O4 C2 1.258(3) . ? O4 Mo1 2.1887(18) . ? O4 Rb1 2.8979(19) 3_565 ? O4 Rb1 3.1286(18) . ? O5 C2 1.238(3) . ? O5 Li1 1.902(5) . ? O5 Li1 2.033(5) 3_665 ? O6 Mo1 2.1950(17) . ? O6 Rb1 3.270(2) 3_565 ? O7 Li2 1.975(5) 2_645 ? O7 Rb1 2.9249(18) 1_545 ? O8 C6 1.248(3) . ? O9 C6 1.239(3) . ? O9 Li2 1.933(5) . ? Li1 O1W 1.898(6) 4_565 ? Li1 O2 1.916(5) 1_655 ? Li1 O5 2.033(5) 3_665 ? Li1 Li1 2.793(9) 3_665 ? Li1 Rb1 3.695(5) 3_665 ? Li1 Rb1 3.857(5) 1_655 ? Li2 O1 1.951(5) 1_655 ? Li2 O3 1.951(4) 2_645 ? Li2 O7 1.975(5) 2_655 ? Li2 Rb1 3.709(4) 2_645 ? Rb1 O4 2.8979(19) 3_565 ? Rb1 O2W 2.918(3) 2 ? Rb1 O7 2.9248(18) 1_565 ? Rb1 O1W 2.926(3) 2_655 ? Rb1 O6 3.270(2) 3_565 ? Rb1 C2 3.530(2) 3_565 ? Rb1 O2 3.5321(19) 3_565 ? Rb1 Mo1 3.6687(4) . ? Rb1 Li1 3.695(5) 3_665 ? Mo1 N1 2.4069(19) . ? Mo1 Rb1 4.1455(4) 3_565 ? C2 C1 1.508(4) . ? C2 Rb1 3.530(2) 3_565 ? N1 C3 1.474(3) . ? N1 C1 1.482(3) . ? N1 C5 1.484(3) . ? C5 C6 1.536(3) . ? 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 O7 C4 O6 123.8(2) . . ? O7 C4 C3 119.3(2) . . ? O6 C4 C3 116.9(2) . . ? Mo1 O1 Li2 171.21(18) . 1_455 ? Mo1 O2 Li1 163.49(19) . 1_455 ? Mo1 O2 Rb1 96.27(7) . . ? Li1 O2 Rb1 99.65(16) 1_455 . ? Mo1 O2 Rb1 97.76(7) . 3_565 ? Li1 O2 Rb1 79.37(15) 1_455 3_565 ? Rb1 O2 Rb1 85.08(5) . 3_565 ? Li1 O1W Rb1 97.69(16) 4_566 2_645 ? Mo1 O3 Li2 163.20(17) . 2_655 ? Mo1 O3 Rb1 93.80(7) . . ? Li2 O3 Rb1 91.12(14) 2_655 . ? C2 O4 Mo1 122.85(16) . . ? C2 O4 Rb1 109.90(16) . 3_565 ? Mo1 O4 Rb1 108.36(7) . 3_565 ? C2 O4 Rb1 130.28(16) . . ? Mo1 O4 Rb1 85.31(6) . . ? Rb1 O4 Rb1 95.38(5) 3_565 . ? C2 O5 Li1 151.0(2) . . ? C2 O5 Li1 117.2(2) . 3_665 ? Li1 O5 Li1 90.4(2) . 3_665 ? C4 O6 Mo1 120.36(16) . . ? C4 O6 Rb1 127.91(16) . 3_565 ? Mo1 O6 Rb1 96.71(6) . 3_565 ? C4 O7 Li2 130.0(2) . 2_645 ? C4 O7 Rb1 133.49(17) . 1_545 ? Li2 O7 Rb1 96.47(14) 2_645 1_545 ? C6 O9 Li2 129.1(2) . . ? O1W Li1 O5 115.2(3) 4_565 . ? O1W Li1 O2 110.6(2) 4_565 1_655 ? O5 Li1 O2 115.6(3) . 1_655 ? O1W Li1 O5 103.8(2) 4_565 3_665 ? O5 Li1 O5 89.6(2) . 3_665 ? O2 Li1 O5 120.3(3) 1_655 3_665 ? O1W Li1 Li1 117.6(3) 4_565 3_665 ? O5 Li1 Li1 46.71(15) . 3_665 ? O2 Li1 Li1 131.4(3) 1_655 3_665 ? O5 Li1 Li1 42.92(14) 3_665 3_665 ? O1W Li1 Rb1 51.71(13) 4_565 3_665 ? O5 Li1 Rb1 165.8(2) . 3_665 ? O2 Li1 Rb1 69.99(14) 1_655 3_665 ? O5 Li1 Rb1 98.61(17) 3_665 3_665 ? Li1 Li1 Rb1 140.3(3) 3_665 3_665 ? O1W Li1 Rb1 122.5(2) 4_565 1_655 ? O5 Li1 Rb1 121.6(2) . 1_655 ? O2 Li1 Rb1 51.03(13) 1_655 1_655 ? O5 Li1 Rb1 69.48(14) 3_665 1_655 ? Li1 Li1 Rb1 95.8(2) 3_665 1_655 ? Rb1 Li1 Rb1 72.35(8) 3_665 1_655 ? O9 Li2 O1 109.7(2) . 1_655 ? O9 Li2 O3 119.3(2) . 2_645 ? O1 Li2 O3 104.5(2) 1_655 2_645 ? O9 Li2 O7 114.1(2) . 2_655 ? O1 Li2 O7 103.0(2) 1_655 2_655 ? O3 Li2 O7 104.7(2) 2_645 2_655 ? O9 Li2 Rb1 119.54(18) . 2_645 ? O1 Li2 Rb1 130.33(18) 1_655 2_645 ? O3 Li2 Rb1 57.15(12) 2_645 2_645 ? O7 Li2 Rb1 51.58(11) 2_655 2_645 ? O4 Rb1 O2W 110.49(6) 3_565 2 ? O4 Rb1 O7 173.54(5) 3_565 1_565 ? O2W Rb1 O7 67.50(6) 2 1_565 ? O4 Rb1 O1W 105.43(6) 3_565 2_655 ? O2W Rb1 O1W 123.19(8) 2 2_655 ? O7 Rb1 O1W 71.88(6) 1_565 2_655 ? O4 Rb1 O2 73.73(5) 3_565 . ? O2W Rb1 O2 110.80(7) 2 . ? O7 Rb1 O2 112.72(5) 1_565 . ? O1W Rb1 O2 120.80(6) 2_655 . ? O4 Rb1 O3 124.44(5) 3_565 . ? O2W Rb1 O3 103.84(6) 2 . ? O7 Rb1 O3 61.82(5) 1_565 . ? O1W Rb1 O3 89.58(6) 2_655 . ? O2 Rb1 O3 53.47(4) . . ? O4 Rb1 O4 84.62(5) 3_565 . ? O2W Rb1 O4 154.24(6) 2 . ? O7 Rb1 O4 99.59(5) 1_565 . ? O1W Rb1 O4 68.86(6) 2_655 . ? O2 Rb1 O4 51.98(5) . . ? O3 Rb1 O4 51.15(5) . . ? O4 Rb1 O6 51.16(5) 3_565 3_565 ? O2W Rb1 O6 92.98(6) 2 3_565 ? O7 Rb1 O6 122.41(5) 1_565 3_565 ? O1W Rb1 O6 76.94(6) 2_655 3_565 ? O2 Rb1 O6 124.80(5) . 3_565 ? O3 Rb1 O6 162.49(5) . 3_565 ? O4 Rb1 O6 112.54(5) . 3_565 ? O4 Rb1 C2 19.57(5) 3_565 3_565 ? O2W Rb1 C2 92.23(7) 2 3_565 ? O7 Rb1 C2 159.72(6) 1_565 3_565 ? O1W Rb1 C2 123.26(6) 2_655 3_565 ? O2 Rb1 C2 72.87(5) . 3_565 ? O3 Rb1 C2 126.30(5) . 3_565 ? O4 Rb1 C2 98.82(5) . 3_565 ? O6 Rb1 C2 56.56(5) 3_565 3_565 ? O4 Rb1 O2 48.53(4) 3_565 3_565 ? O2W Rb1 O2 141.17(6) 2 3_565 ? O7 Rb1 O2 129.05(5) 1_565 3_565 ? O1W Rb1 O2 57.17(6) 2_655 3_565 ? O2 Rb1 O2 94.92(5) . 3_565 ? O3 Rb1 O2 114.90(4) . 3_565 ? O4 Rb1 O2 64.40(4) . 3_565 ? O6 Rb1 O2 48.20(4) 3_565 3_565 ? C2 Rb1 O2 67.45(5) 3_565 3_565 ? O4 Rb1 Mo1 96.20(4) 3_565 . ? O2W Rb1 Mo1 118.75(6) 2 . ? O7 Rb1 Mo1 90.06(4) 1_565 . ? O1W Rb1 Mo1 98.84(5) 2_655 . ? O2 Rb1 Mo1 28.21(3) . . ? O3 Rb1 Mo1 28.24(3) . . ? O4 Rb1 Mo1 36.48(3) . . ? O6 Rb1 Mo1 142.44(3) 3_565 . ? C2 Rb1 Mo1 99.77(4) 3_565 . ? O2 Rb1 Mo1 97.78(3) 3_565 . ? O4 Rb1 Li1 78.30(8) 3_565 3_665 ? O2W Rb1 Li1 149.46(10) 2 3_665 ? O7 Rb1 Li1 100.38(8) 1_565 3_665 ? O1W Rb1 Li1 30.60(9) 2_655 3_665 ? O2 Rb1 Li1 99.73(9) . 3_665 ? O3 Rb1 Li1 93.39(8) . 3_665 ? O4 Rb1 Li1 51.74(8) . 3_665 ? O6 Rb1 Li1 69.32(8) 3_565 3_665 ? C2 Rb1 Li1 97.67(8) 3_565 3_665 ? O2 Rb1 Li1 30.64(8) 3_565 3_665 ? Mo1 Rb1 Li1 88.00(8) . 3_665 ? O1 Mo1 O3 104.67(9) . . ? O1 Mo1 O2 107.15(9) . . ? O3 Mo1 O2 105.38(8) . . ? O1 Mo1 O4 159.66(8) . . ? O3 Mo1 O4 85.87(8) . . ? O2 Mo1 O4 86.12(8) . . ? O1 Mo1 O6 89.01(9) . . ? O3 Mo1 O6 155.52(8) . . ? O2 Mo1 O6 89.31(8) . . ? O4 Mo1 O6 75.51(7) . . ? O1 Mo1 N1 89.74(8) . . ? O3 Mo1 N1 88.23(7) . . ? O2 Mo1 N1 154.30(8) . . ? O4 Mo1 N1 72.99(6) . . ? O6 Mo1 N1 71.35(6) . . ? O1 Mo1 Rb1 142.10(7) . . ? O3 Mo1 Rb1 57.96(6) . . ? O2 Mo1 Rb1 55.52(6) . . ? O4 Mo1 Rb1 58.20(5) . . ? O6 Mo1 Rb1 120.85(5) . . ? N1 Mo1 Rb1 120.16(5) . . ? O1 Mo1 Rb1 134.23(7) . 3_565 ? O3 Mo1 Rb1 120.73(7) . 3_565 ? O2 Mo1 Rb1 57.59(6) . 3_565 ? O4 Mo1 Rb1 41.56(5) . 3_565 ? O6 Mo1 Rb1 51.57(5) . 3_565 ? N1 Mo1 Rb1 96.74(5) . 3_565 ? Rb1 Mo1 Rb1 69.288(8) . 3_565 ? O5 C2 O4 122.1(2) . . ? O5 C2 C1 119.2(2) . . ? O4 C2 C1 118.6(2) . . ? O5 C2 Rb1 86.86(15) . 3_565 ? O4 C2 Rb1 50.53(13) . 3_565 ? C1 C2 Rb1 136.89(18) . 3_565 ? C3 N1 C1 112.6(3) . . ? C3 N1 C5 109.1(2) . . ? C1 N1 C5 111.1(2) . . ? C3 N1 Mo1 106.15(15) . . ? C1 N1 Mo1 108.83(15) . . ? C5 N1 Mo1 108.88(14) . . ? N1 C5 C6 117.0(2) . . ? O9 C6 O8 125.4(2) . . ? O9 C6 C5 120.4(2) . . ? O8 C6 C5 114.1(2) . . ? N1 C1 C2 114.0(2) . . ? N1 C3 C4 113.6(2) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment 'Data for 3.cif' data_y _database_code_depnum_ccdc_archive 'CCDC 902738' #TrackingRef 'Data for 3.cif' _audit_creation_date 2011-10-13T12:59:46-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C12 H12 Cs2 Li3 Mo2 N2 O20, Li O2' _chemical_formula_sum 'C12 H12 Cs2 Li4 Mo2 N2 O22' _chemical_formula_weight 1021.7 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c' _symmetry_space_group_name_Hall '-P 2yc' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 14.0195(13) _cell_length_b 13.7541(13) _cell_length_c 7.7115(7) _cell_angle_alpha 90 _cell_angle_beta 102.829(2) _cell_angle_gamma 90 _cell_volume 1449.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.34 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.431 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_unetI/netI 0.0242 _diffrn_reflns_number 20606 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 31.37 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.885 _reflns_number_total 4789 _reflns_number_gt 3646 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^)+(0.0430P)^2^+3.1474P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4789 _refine_ls_number_parameters 229 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.032 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.74 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.142 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 C1 C 0.3657(3) 0.2153(4) 0.5670(6) 0.0402(10) Uani 1 1 d D . . C2 C 0.3553(3) 0.2987(3) 0.4371(5) 0.0290(7) Uani 1 1 d . . . C3 C 0.2241(3) 0.1144(3) 0.5799(5) 0.0298(8) Uani 1 1 d . . . C4 C 0.1588(3) 0.1374(3) 0.3996(4) 0.0261(7) Uani 1 1 d . . . C5 C 0.3143(3) 0.1965(3) 0.8485(4) 0.0286(8) Uani 1 1 d . . . C6 C 0.3903(3) 0.1173(3) 0.9244(5) 0.0265(7) Uani 1 1 d . . . N1 N 0.2819(2) 0.2017(2) 0.6523(3) 0.0213(5) Uani 1 1 d . . . O1 O 0.2382(2) 0.4066(2) 0.7446(3) 0.0322(6) Uani 1 1 d . . . O2 O 0.09647(19) 0.41738(18) 0.4316(3) 0.0273(5) Uani 1 1 d . . . O1W O 0.0661(3) 0.1025(2) 0.9386(4) 0.0525(9) Uani 1 1 d . . . O3 O 0.0902(2) 0.27323(19) 0.6784(3) 0.0294(5) Uani 1 1 d . . . O2W O 0.3882(6) 0.4670(4) 0.1152(11) 0.143(3) Uani 1 1 d . . . O4 O 0.2863(2) 0.3587(2) 0.4302(4) 0.0324(6) Uani 1 1 d . . . O5 O 0.1423(2) 0.22677(18) 0.3619(3) 0.0284(5) Uani 1 1 d . . . O6 O 0.1250(2) 0.0696(2) 0.3001(3) 0.0380(7) Uani 1 1 d . . . O7 O 0.4177(3) 0.3072(2) 0.3464(5) 0.0519(9) Uani 1 1 d . . . O8 O 0.4059(3) 0.0521(2) 0.8261(4) 0.0468(8) Uani 1 1 d . . . O9 O 0.4296(2) 0.1274(2) 1.0873(3) 0.0320(6) Uani 1 1 d . . . Mo1 Mo 0.16962(2) 0.33572(2) 0.57341(3) 0.01936(8) Uani 1 1 d . . . Cs1 Cs 0.119242(19) 0.372506(18) 1.05153(3) 0.03199(8) Uani 1 1 d . . . Li1 Li 0 0.1824(6) 0.75 0.0282(18) Uani 1 2 d S . . Li2 Li 0.5 0.2195(7) 1.25 0.0285(18) Uani 1 2 d S . . Li3 Li 0.5 -0.0260(6) 0.75 0.0294(18) Uani 1 2 d S . . Li4 Li 0.4436(9) 0.5542(12) 0.2837(18) 0.035(3) Uani 0.5 1 d P . . H1A H 0.426(5) 0.232(4) 0.663(8) 0.070(19) Uiso 1 1 d . . . H1B H 0.379(5) 0.156(3) 0.507(8) 0.08(2) Uiso 1 1 d D . . H3A H 0.269(3) 0.061(3) 0.573(6) 0.030(11) Uiso 1 1 d . . . H3B H 0.184(4) 0.100(4) 0.668(7) 0.040(13) Uiso 1 1 d . . . H5A H 0.338(4) 0.250(4) 0.890(7) 0.042(14) Uiso 1 1 d . . . H5B H 0.253(3) 0.189(3) 0.897(6) 0.024(10) 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 C1 0.030(2) 0.053(3) 0.041(2) 0.015(2) 0.0152(18) 0.015(2) C2 0.0288(19) 0.0303(18) 0.0314(17) -0.0071(14) 0.0142(14) 0.0012(15) C3 0.035(2) 0.0219(16) 0.0264(17) -0.0007(13) -0.0057(15) 0.0049(15) C4 0.031(2) 0.0276(16) 0.0184(14) -0.0010(12) 0.0029(13) 0.0011(14) C5 0.034(2) 0.0307(18) 0.0178(14) -0.0022(13) -0.0005(14) 0.0080(16) C6 0.0242(19) 0.0278(17) 0.0252(15) 0.0031(13) 0.0003(13) 0.0031(13) N1 0.0211(14) 0.0258(13) 0.0169(11) 0.0005(10) 0.0040(10) 0.0035(11) O1 0.0352(15) 0.0339(14) 0.0273(12) -0.0061(11) 0.0067(11) -0.0070(12) O2 0.0309(14) 0.0261(12) 0.0259(11) 0.0039(10) 0.0083(10) 0.0061(11) O1W 0.089(3) 0.0373(16) 0.0290(14) 0.0080(12) 0.0070(16) 0.0210(17) O3 0.0292(14) 0.0299(13) 0.0319(13) 0.0016(10) 0.0124(11) -0.0011(11) O2W 0.149(6) 0.071(4) 0.185(7) 0.052(4) -0.020(5) 0.043(4) O4 0.0321(15) 0.0342(14) 0.0343(14) 0.0048(11) 0.0146(12) 0.0081(12) O5 0.0381(15) 0.0239(12) 0.0199(11) -0.0007(9) -0.0007(10) 0.0047(11) O6 0.0542(19) 0.0275(13) 0.0266(13) -0.0042(10) -0.0029(12) -0.0029(13) O7 0.056(2) 0.0414(17) 0.074(2) 0.0100(16) 0.0486(19) 0.0119(16) O8 0.051(2) 0.0445(17) 0.0373(15) -0.0069(13) -0.0060(14) 0.0270(15) O9 0.0331(15) 0.0331(14) 0.0239(12) 0.0036(10) -0.0062(11) 0.0015(11) Mo1 0.02030(15) 0.02056(14) 0.01824(13) -0.00014(9) 0.00645(10) 0.00178(10) Cs1 0.03898(16) 0.03563(14) 0.02229(11) 0.00208(8) 0.00881(9) 0.00397(10) Li1 0.037(5) 0.022(4) 0.027(4) 0 0.011(4) 0 Li2 0.028(5) 0.031(4) 0.030(4) 0 0.012(3) 0 Li3 0.028(5) 0.025(4) 0.031(4) 0 -0.003(3) 0 Li4 0.010(5) 0.060(9) 0.037(7) 0.021(6) 0.010(5) 0.016(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 C1 N1 1.480(5) . ? C1 C2 1.509(6) . ? C2 O7 1.240(5) . ? C2 O4 1.264(5) . ? C3 N1 1.486(5) . ? C3 C4 1.518(5) . ? C4 O6 1.234(4) . ? C4 O5 1.272(4) . ? C5 N1 1.482(4) . ? C5 C6 1.546(5) . ? C6 O8 1.225(5) . ? C6 O9 1.262(4) . ? N1 Mo1 2.413(3) . ? O1 Mo1 1.748(3) . ? O1 Cs1 3.218(3) . ? O1 Cs1 3.623(3) 4_565 ? O2 Mo1 1.735(2) . ? O2 Cs1 3.030(3) 4_565 ? O2 Cs1 3.080(2) 1_554 ? O2 Cs1 3.117(3) 2_556 ? O1W Li1 1.893(6) . ? O3 Mo1 1.742(3) . ? O3 Li1 1.942(6) . ? O3 Cs1 3.129(3) . ? O3 Cs1 3.364(3) 2_556 ? O2W Li4 1.812(18) . ? O2W Li4 2.606(14) 2_655 ? O4 Mo1 2.190(3) . ? O4 Cs1 3.318(3) 1_554 ? O5 Mo1 2.185(2) . ? O5 Cs1 3.083(2) 1_554 ? O7 Li2 1.929(7) 1_554 ? O8 Li3 1.892(6) . ? O9 Li2 1.899(7) . ? O9 Li3 1.986(7) 3_657 ? Mo1 Cs1 3.9377(5) . ? Mo1 Cs1 3.9610(5) 1_554 ? Mo1 Cs1 3.9814(5) 2_556 ? Mo1 Cs1 4.0717(5) 4_565 ? Cs1 O2 3.030(3) 4_566 ? Cs1 O2 3.080(2) 1_556 ? Cs1 O5 3.083(2) 1_556 ? Cs1 O2 3.117(3) 2_556 ? Cs1 O4 3.318(3) 1_556 ? Cs1 O3 3.364(3) 2_556 ? Cs1 O1 3.623(3) 4_566 ? Cs1 Li1 3.648(6) . ? Cs1 Mo1 3.9610(5) 1_556 ? Li1 O1W 1.893(6) 2_556 ? Li1 O3 1.942(6) 2_556 ? Li1 Cs1 3.648(6) 2_556 ? Li2 O9 1.899(7) 2_657 ? Li2 O7 1.929(7) 2_656 ? Li2 O7 1.929(7) 1_556 ? Li2 Li3 2.662(13) 3_657 ? Li3 O8 1.892(6) 2_656 ? Li3 O9 1.986(7) 4 ? Li3 O9 1.986(7) 3_657 ? Li3 Li2 2.662(13) 3_657 ? Li4 Li4 1.77(2) 2_655 ? Li4 O2W 2.606(14) 2_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_3 _geom_angle_publ_flag N1 C1 C2 115.0(3) . . ? O7 C2 O4 123.0(4) . . ? O7 C2 C1 118.0(4) . . ? O4 C2 C1 119.0(3) . . ? N1 C3 C4 110.1(3) . . ? O6 C4 O5 124.3(3) . . ? O6 C4 C3 118.8(3) . . ? O5 C4 C3 116.9(3) . . ? N1 C5 C6 116.7(3) . . ? O8 C6 O9 126.8(3) . . ? O8 C6 C5 119.0(3) . . ? O9 C6 C5 114.2(3) . . ? C1 N1 C5 111.5(3) . . ? C1 N1 C3 110.8(3) . . ? C5 N1 C3 111.3(3) . . ? C1 N1 Mo1 109.2(2) . . ? C5 N1 Mo1 109.2(2) . . ? C3 N1 Mo1 104.6(2) . . ? Mo1 O1 Cs1 100.73(11) . . ? Mo1 O1 Cs1 91.80(11) . 4_565 ? Cs1 O1 Cs1 99.08(8) . 4_565 ? Mo1 O2 Cs1 114.67(12) . 4_565 ? Mo1 O2 Cs1 107.37(11) . 1_554 ? Cs1 O2 Cs1 117.10(8) 4_565 1_554 ? Mo1 O2 Cs1 106.77(11) . 2_556 ? Cs1 O2 Cs1 102.33(7) 4_565 2_556 ? Cs1 O2 Cs1 107.85(8) 1_554 2_556 ? Mo1 O3 Li1 166.7(2) . . ? Mo1 O3 Cs1 104.23(11) . . ? Li1 O3 Cs1 88.80(15) . . ? Mo1 O3 Cs1 97.36(10) . 2_556 ? Li1 O3 Cs1 82.18(15) . 2_556 ? Cs1 O3 Cs1 103.17(7) . 2_556 ? Li4 O2W Li4 42.7(6) . 2_655 ? C2 O4 Mo1 122.4(3) . . ? C2 O4 Cs1 117.3(2) . 1_554 ? Mo1 O4 Cs1 89.54(9) . 1_554 ? C4 O5 Mo1 119.9(2) . . ? C4 O5 Cs1 142.0(2) . 1_554 ? Mo1 O5 Cs1 95.99(9) . 1_554 ? C2 O7 Li2 135.7(4) . 1_554 ? C6 O8 Li3 147.1(3) . . ? C6 O9 Li2 141.2(3) . . ? C6 O9 Li3 126.7(3) . 3_657 ? Li2 O9 Li3 86.5(3) . 3_657 ? O2 Mo1 O3 105.24(13) . . ? O2 Mo1 O1 105.32(13) . . ? O3 Mo1 O1 103.05(13) . . ? O2 Mo1 O5 89.56(11) . . ? O3 Mo1 O5 89.10(12) . . ? O1 Mo1 O5 157.24(12) . . ? O2 Mo1 O4 89.52(11) . . ? O3 Mo1 O4 158.68(11) . . ? O1 Mo1 O4 87.31(12) . . ? O5 Mo1 O4 75.48(11) . . ? O2 Mo1 N1 156.14(10) . . ? O3 Mo1 N1 87.41(11) . . ? O1 Mo1 N1 90.96(12) . . ? O5 Mo1 N1 70.16(9) . . ? O4 Mo1 N1 73.67(10) . . ? O2 Mo1 Cs1 107.66(8) . . ? O3 Mo1 Cs1 50.38(9) . . ? O1 Mo1 Cs1 53.42(9) . . ? O5 Mo1 Cs1 138.49(7) . . ? O4 Mo1 Cs1 139.73(8) . . ? N1 Mo1 Cs1 96.02(6) . . ? O2 Mo1 Cs1 47.92(8) . 1_554 ? O3 Mo1 Cs1 123.15(9) . 1_554 ? O1 Mo1 Cs1 129.82(9) . 1_554 ? O5 Mo1 Cs1 50.73(7) . 1_554 ? O4 Mo1 Cs1 56.89(8) . 1_554 ? N1 Mo1 Cs1 108.23(6) . 1_554 ? Cs1 Mo1 Cs1 155.006(11) . 1_554 ? O2 Mo1 Cs1 48.57(9) . 2_556 ? O3 Mo1 Cs1 56.92(9) . 2_556 ? O1 Mo1 Cs1 118.14(10) . 2_556 ? O5 Mo1 Cs1 84.62(7) . 2_556 ? O4 Mo1 Cs1 133.86(7) . 2_556 ? N1 Mo1 Cs1 136.88(7) . 2_556 ? Cs1 Mo1 Cs1 79.978(8) . 2_556 ? Cs1 Mo1 Cs1 78.203(8) 1_554 2_556 ? O2 Mo1 Cs1 42.54(9) . 4_565 ? O3 Mo1 Cs1 112.49(9) . 4_565 ? O1 Mo1 Cs1 62.80(10) . 4_565 ? O5 Mo1 Cs1 130.16(6) . 4_565 ? O4 Mo1 Cs1 88.79(7) . 4_565 ? N1 Mo1 Cs1 149.42(7) . 4_565 ? Cs1 Mo1 Cs1 81.178(7) . 4_565 ? Cs1 Mo1 Cs1 80.899(7) 1_554 4_565 ? Cs1 Mo1 Cs1 72.959(7) 2_556 4_565 ? O2 Cs1 O2 94.20(5) 4_566 1_556 ? O2 Cs1 O5 147.45(6) 4_566 1_556 ? O2 Cs1 O5 53.62(6) 1_556 1_556 ? O2 Cs1 O2 77.67(7) 4_566 2_556 ? O2 Cs1 O2 67.30(8) 1_556 2_556 ? O5 Cs1 O2 91.82(7) 1_556 2_556 ? O2 Cs1 O3 98.75(7) 4_566 . ? O2 Cs1 O3 160.50(7) 1_556 . ? O5 Cs1 O3 113.58(7) 1_556 . ? O2 Cs1 O3 101.27(7) 2_556 . ? O2 Cs1 O1 70.92(7) 4_566 . ? O2 Cs1 O1 148.29(7) 1_556 . ? O5 Cs1 O1 133.11(7) 1_556 . ? O2 Cs1 O1 131.91(7) 2_556 . ? O3 Cs1 O1 50.96(7) . . ? O2 Cs1 O4 109.22(7) 4_566 1_556 ? O2 Cs1 O4 51.40(7) 1_556 1_556 ? O5 Cs1 O4 49.29(7) 1_556 1_556 ? O2 Cs1 O4 118.43(6) 2_556 1_556 ? O3 Cs1 O4 134.97(7) . 1_556 ? O1 Cs1 O4 106.01(7) . 1_556 ? O2 Cs1 O3 101.88(7) 4_566 2_556 ? O2 Cs1 O3 108.67(7) 1_556 2_556 ? O5 Cs1 O3 94.24(7) 1_556 2_556 ? O2 Cs1 O3 50.30(6) 2_556 2_556 ? O3 Cs1 O3 54.40(8) . 2_556 ? O1 Cs1 O3 101.87(7) . 2_556 ? O4 Cs1 O3 143.46(7) 1_556 2_556 ? O2 Cs1 O1 48.18(6) 4_566 4_566 ? O2 Cs1 O1 64.95(7) 1_556 4_566 ? O5 Cs1 O1 105.48(6) 1_556 4_566 ? O2 Cs1 O1 100.32(6) 2_556 4_566 ? O3 Cs1 O1 134.26(6) . 4_566 ? O1 Cs1 O1 85.04(6) . 4_566 ? O4 Cs1 O1 61.04(6) 1_556 4_566 ? O3 Cs1 O1 145.62(6) 2_556 4_566 ? O2 Cs1 Li1 119.12(11) 4_566 . ? O2 Cs1 Li1 128.35(7) 1_556 . ? O5 Cs1 Li1 89.03(10) 1_556 . ? O2 Cs1 Li1 81.78(6) 2_556 . ? O3 Cs1 Li1 32.16(6) . . ? O1 Cs1 Li1 82.80(6) . . ? O4 Cs1 Li1 130.83(11) 1_556 . ? O3 Cs1 Li1 31.83(7) 2_556 . ? O1 Cs1 Li1 165.20(9) 4_566 . ? O2 Cs1 Mo1 82.26(5) 4_566 . ? O2 Cs1 Mo1 174.09(5) 1_556 . ? O5 Cs1 Mo1 129.32(5) 1_556 . ? O2 Cs1 Mo1 116.23(5) 2_556 . ? O3 Cs1 Mo1 25.40(5) . . ? O1 Cs1 Mo1 25.85(5) . . ? O4 Cs1 Mo1 125.34(5) 1_556 . ? O3 Cs1 Mo1 76.78(4) 2_556 . ? O1 Cs1 Mo1 109.30(4) 4_566 . ? Li1 Cs1 Mo1 57.53(4) . . ? O2 Cs1 Mo1 114.52(5) 4_566 1_556 ? O2 Cs1 Mo1 24.72(5) 1_556 1_556 ? O5 Cs1 Mo1 33.28(5) 1_556 1_556 ? O2 Cs1 Mo1 86.48(5) 2_556 1_556 ? O3 Cs1 Mo1 146.73(5) . 1_556 ? O1 Cs1 Mo1 139.57(5) . 1_556 ? O4 Cs1 Mo1 33.57(5) 1_556 1_556 ? O3 Cs1 Mo1 114.93(4) 2_556 1_556 ? O1 Cs1 Mo1 74.20(4) 4_566 1_556 ? Li1 Cs1 Mo1 120.61(8) . 1_556 ? Mo1 Cs1 Mo1 155.006(11) . 1_556 ? O1W Li1 O1W 109.0(5) 2_556 . ? O1W Li1 O3 110.69(16) 2_556 2_556 ? O1W Li1 O3 113.16(14) . 2_556 ? O1W Li1 O3 113.16(14) 2_556 . ? O1W Li1 O3 110.69(16) . . ? O3 Li1 O3 100.0(4) 2_556 . ? O1W Li1 Cs1 169.3(3) 2_556 . ? O1W Li1 Cs1 81.35(16) . . ? O3 Li1 Cs1 65.99(19) 2_556 . ? O3 Li1 Cs1 59.04(18) . . ? O1W Li1 Cs1 81.35(16) 2_556 2_556 ? O1W Li1 Cs1 169.3(3) . 2_556 ? O3 Li1 Cs1 59.04(18) 2_556 2_556 ? O3 Li1 Cs1 65.99(19) . 2_556 ? Cs1 Li1 Cs1 88.45(19) . 2_556 ? O9 Li2 O9 96.3(4) 2_657 . ? O9 Li2 O7 113.85(16) 2_657 2_656 ? O9 Li2 O7 115.48(14) . 2_656 ? O9 Li2 O7 115.48(14) 2_657 1_556 ? O9 Li2 O7 113.85(16) . 1_556 ? O7 Li2 O7 102.6(5) 2_656 1_556 ? O9 Li2 Li3 48.1(2) 2_657 3_657 ? O9 Li2 Li3 48.1(2) . 3_657 ? O7 Li2 Li3 128.7(2) 2_656 3_657 ? O7 Li2 Li3 128.7(2) 1_556 3_657 ? O8 Li3 O8 110.9(5) . 2_656 ? O8 Li3 O9 108.14(15) . 4 ? O8 Li3 O9 119.04(15) 2_656 4 ? O8 Li3 O9 119.04(15) . 3_657 ? O8 Li3 O9 108.14(15) 2_656 3_657 ? O9 Li3 O9 90.8(4) 4 3_657 ? O8 Li3 Li2 124.6(2) . 3_657 ? O8 Li3 Li2 124.6(2) 2_656 3_657 ? O9 Li3 Li2 45.40(19) 4 3_657 ? O9 Li3 Li2 45.40(19) 3_657 3_657 ? Li4 Li4 O2W 93.3(8) 2_655 . ? Li4 Li4 O2W 44.0(6) 2_655 2_655 ? O2W Li4 O2W 97.1(6) . 2_655 ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF