data_general _publ_contact_author_name 'Dr Salete S. Balula ' _publ_contact_author_address ; REQUIMTE & Departamento de Qu\'imica e Bioqu\'imica Faculdade de Ci\^encias Universidade do Porto 4169-007 Porto Portugal ; _publ_contact_author_email 'sbalula@fc.up.pt.pt' _publ_contact_author_fax '+351 220402576' _publ_contact_author_phone '+351 220402659' _journal_name_full 'ACS Catalysis' loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Balula, Salete S.' . ; REQUIMTE & Departamento de Qu\'imica e Bioqu\'imica Faculdade de Ci\^encias Universidade do Porto 4169-007 Porto Portugal ; 'Cunha-Silva, Lu\'is' . ; REQUIMTE & Departamento de Qu\'imica e Bioqu\'imica Faculdade de Ci\^encias Universidade do Porto 4169-007 Porto Portugal ; 'Santos, Isabel C. M. S.' . ; Departamento de Qu\'imica QOPNA Universidade de Aveiro 3810-193 Aveiro Portugal ; 'Estrada, Ana C.' . ; Departamento de Qu\'imica CICECO Universidade de Aveiro 3810-193 Aveiro Portugal ; 'Fernandes, A. C.' . ; Departamento de Qu\'imica e Bioqu\'imica CQB, Faculdade de Ci\^encias Universidade de Lisboa 1749-016 Lisboa Portugal ; 'Cavaleiro, Jos\'e A. S.' . ; Departamento de Qu\'imica QOPNA Universidade de Aveiro 3810-193 Aveiro Portugal ; 'Pires, Jo\~ao' . ; Departamento de Qu\'imica e Bioqu\'imica CQB, Faculdade de Ci\^encias Universidade de Lisboa 1749-016 Lisboa Portugal ; 'Freire, Cristina' . ; REQUIMTE & Departamento de Qu\'imica e Bioqu\'imica Faculdade de Ci\^encias Universidade do Porto 4169-007 Porto Portugal ; 'Cavaleiro, Ana M. V.' . ; Departamento de Qu\'imica CICECO Universidade de Aveiro 3810-193 Aveiro Portugal ; data_sb0310 # ========================================================================== # _audit_creation_method 'SHELXL-97, manual editing plus enCIFer' _audit_creation_date '12 January 2012' # ========================================================================== # #============================================================================# # GENERAL AND CHEMICAL DATA # #============================================================================# _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'K4, H2, Si W11 Co H2 O40, 22(H20)' _chemical_formula_sum 'Co H48 K4 O62 Si W11' _chemical_formula_weight 3306.15 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #============================================================================# # CRYSTAL DATA # #============================================================================# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/m n c' _symmetry_space_group_name_Hall '-P 4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x-1/2, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 14.1182(7) _cell_length_b 14.1182(7) _cell_length_c 12.4604(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2483.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3245 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 25.38 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2950 _exptl_absorpt_coefficient_mu 26.184 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0030 _exptl_absorpt_correction_T_max 0.0120 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1997) ; _exptl_special_details ; ? ; #============================================================================# # EXPERIMENTAL DATA # #============================================================================# _diffrn_ambient_temperature 150(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 'Bruker X8 Kappa CCD APEX II' _diffrn_measurement_method 'omega/phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11494 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.36 _diffrn_reflns_theta_max 26.36 _reflns_number_total 1333 _reflns_number_gt 1247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'APEX2 ' _computing_data_reduction 'SAINT+ (Bruker, 1997-2005)' _computing_structure_solution 'SHELXTL (Bruker 2001)' _computing_structure_refinement 'SHELXTL ' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material 'SHELXTL ' #============================================================================# # REFINEMENT DATA # #============================================================================# _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^)+(0.0324P)^2^+97.3676P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1333 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #============================================================================# # ATOMIC COORDINATES AND DISPLACEMENT 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 W1 W 0.61072(4) 0.63756(3) 0.70034(4) 0.01940(18) Uani 0.92 1 d P . . Co1 Co 0.61072(4) 0.63756(3) 0.70034(4) 0.01940(18) Uani 0.08 1 d P . . W2 W 0.74719(5) 0.52587(6) 0.5000 0.0249(2) Uani 0.92 2 d SP . . Co2 Co 0.74719(5) 0.52587(6) 0.5000 0.0249(2) Uani 0.08 2 d SP . . O4 O 0.7131(12) 0.6170(7) 0.6038(11) 0.075(5) Uani 1 1 d . . . Si1 Si 0.5000 0.5000 0.5000 0.0088(14) Uani 1 8 d S . . K1 K 0.7937(3) 0.2537(3) 0.5000 0.0347(10) Uani 1 2 d S . . O11 O 0.8909(11) 0.6091(11) 0.7500 0.117(11) Uani 1 2 d S . . O9 O 0.9070(8) 0.4070(8) 0.2500 0.071(6) Uani 1 2 d S . . O10 O 0.5585(14) 0.3168(14) 0.0000 0.071(6) Uani 1 2 d S . . O2 O 0.6298(12) 0.5144(7) 0.7536(13) 0.087(6) Uani 1 1 d . . . O1 O 0.6610(9) 0.7024(8) 0.7975(7) 0.049(3) Uani 1 1 d . . . O5 O 0.8676(10) 0.5407(12) 0.5000 0.058(5) Uani 1 2 d S . . O3 O 0.5711(7) 0.7334(11) 0.6040(10) 0.073(5) Uani 1 1 d . . . O6 O 0.5097(10) 0.4050(10) 0.4232(11) 0.065(3) Uani 1 1 d . . . O8 O 0.5000 0.5000 0.056(3) 0.116(13) Uani 1 4 d S . . O7 O 0.962(2) 0.351(2) 0.540(8) 0.19(6) Uani 0.50 1 d P . . 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 W1 0.0299(3) 0.0245(3) 0.0038(2) -0.00299(17) -0.00180(18) -0.01350(19) Co1 0.0299(3) 0.0245(3) 0.0038(2) -0.00299(17) -0.00180(18) -0.01350(19) W2 0.0162(4) 0.0320(4) 0.0264(4) 0.000 0.000 -0.0024(3) Co2 0.0162(4) 0.0320(4) 0.0264(4) 0.000 0.000 -0.0024(3) O4 0.136(13) 0.023(5) 0.065(8) 0.009(5) 0.081(9) 0.009(6) Si1 0.010(2) 0.010(2) 0.007(3) 0.000 0.000 0.000 K1 0.048(2) 0.045(2) 0.0115(16) 0.000 0.000 0.028(2) O11 0.113(13) 0.113(13) 0.13(2) -0.078(15) -0.078(15) 0.054(15) O9 0.040(5) 0.040(5) 0.133(18) -0.030(8) 0.030(8) -0.001(7) O10 0.059(12) 0.068(12) 0.086(15) 0.000 0.000 -0.015(10) O2 0.143(13) 0.024(5) 0.093(10) 0.016(6) 0.103(10) 0.017(7) O1 0.077(8) 0.058(7) 0.012(4) -0.005(4) -0.004(5) -0.042(6) O5 0.018(7) 0.053(10) 0.103(15) 0.000 0.000 -0.004(6) O3 0.029(5) 0.140(13) 0.050(7) 0.079(8) -0.008(5) -0.010(7) O6 0.069(8) 0.069(8) 0.058(7) 0.000(7) 0.005(7) 0.001(7) O8 0.14(2) 0.14(2) 0.07(2) 0.000 0.000 0.000 O7 0.058(16) 0.067(17) 0.46(19) 0.10(5) 0.08(5) 0.003(14) #============================================================================# # 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 W1 O1 1.676(9) . ? W1 O2 1.881(11) . ? W1 O2 1.891(12) 2_655 ? W1 O3 1.893(10) . ? W1 O4 1.903(11) . ? W1 O6 2.371(15) 9_666 ? W1 O6 2.383(14) 12_656 ? W1 K1 3.842(3) 2_655 ? W2 O5 1.713(14) . ? W2 O4 1.887(11) 11_556 ? W2 O4 1.887(11) . ? W2 O3 1.895(10) 10_566 ? W2 O3 1.895(10) 4_565 ? W2 O6 2.363(14) 2_655 ? W2 O6 2.363(14) 12_656 ? W2 K1 3.781(5) 2_655 ? W2 K1 3.899(4) . ? O4 K1 2.849(11) 2_655 ? Si1 O6 1.654(14) 9_666 ? Si1 O6 1.654(14) . ? Si1 O6 1.654(14) 4_565 ? Si1 O6 1.654(14) 12_656 ? Si1 O6 1.654(14) 3_665 ? Si1 O6 1.654(14) 2_655 ? Si1 O6 1.654(14) 10_566 ? Si1 O6 1.654(14) 11_556 ? K1 O1 2.702(9) 13_755 ? K1 O1 2.702(9) 6_646 ? K1 O10 2.77(2) 7_545 ? K1 O7 2.80(4) . ? K1 O7 2.80(4) 11_556 ? K1 O4 2.849(11) 10_566 ? K1 O4 2.849(11) 4_565 ? K1 O3 2.920(11) 4_565 ? K1 O3 2.920(11) 10_566 ? K1 W2 3.781(5) 10_566 ? K1 Co2 3.781(5) 10_566 ? K1 Co1 3.842(3) 10_566 ? O10 K1 2.77(2) 7_545 ? O2 Co1 1.891(12) 4_565 ? O2 W1 1.891(12) 4_565 ? O1 K1 2.702(9) 13_766 ? O3 Co2 1.895(10) 2_655 ? O3 W2 1.895(10) 2_655 ? O3 K1 2.920(11) 2_655 ? O6 Co2 2.363(14) 10_566 ? O6 W2 2.363(14) 10_566 ? O6 W1 2.371(14) 9_666 ? O6 Co1 2.371(14) 9_666 ? O6 Co1 2.383(14) 10_566 ? O6 W1 2.383(14) 10_566 ? O8 O8 1.41(7) 9_665 ? O7 O7 1.0(2) 11_556 ? 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 W1 O2 100.9(7) . . ? O1 W1 O2 100.0(7) . 2_655 ? O2 W1 O2 87.5(8) . 2_655 ? O1 W1 O3 101.1(6) . . ? O2 W1 O3 158.0(8) . . ? O2 W1 O3 89.3(5) 2_655 . ? O1 W1 O4 102.6(7) . . ? O2 W1 O4 88.5(5) . . ? O2 W1 O4 157.4(8) 2_655 . ? O3 W1 O4 86.1(5) . . ? O1 W1 O6 155.7(6) . 9_666 ? O2 W1 O6 95.6(7) . 9_666 ? O2 W1 O6 62.8(6) 2_655 9_666 ? O3 W1 O6 63.7(5) . 9_666 ? O4 W1 O6 95.5(6) . 9_666 ? O1 W1 O6 156.9(6) . 12_656 ? O2 W1 O6 62.7(6) . 12_656 ? O2 W1 O6 95.5(7) 2_655 12_656 ? O3 W1 O6 96.0(6) . 12_656 ? O4 W1 O6 63.1(5) . 12_656 ? O6 W1 O6 47.3(6) 9_666 12_656 ? O1 W1 K1 86.8(3) . 2_655 ? O2 W1 K1 133.5(3) . 2_655 ? O2 W1 K1 136.6(3) 2_655 2_655 ? O3 W1 K1 47.6(3) . 2_655 ? O4 W1 K1 45.4(3) . 2_655 ? O6 W1 K1 94.6(3) 9_666 2_655 ? O6 W1 K1 93.5(3) 12_656 2_655 ? O5 W2 O4 99.8(7) . 11_556 ? O5 W2 O4 99.8(7) . . ? O4 W2 O4 86.5(8) 11_556 . ? O5 W2 O3 101.0(6) . 10_566 ? O4 W2 O3 89.9(4) 11_556 10_566 ? O4 W2 O3 159.3(7) . 10_566 ? O5 W2 O3 101.0(6) . 4_565 ? O4 W2 O3 159.3(7) 11_556 4_565 ? O4 W2 O3 89.9(4) . 4_565 ? O3 W2 O3 86.3(7) 10_566 4_565 ? O5 W2 O6 156.1(3) . 2_655 ? O4 W2 O6 63.7(6) 11_556 2_655 ? O4 W2 O6 96.4(7) . 2_655 ? O3 W2 O6 63.9(5) 10_566 2_655 ? O3 W2 O6 96.5(6) 4_565 2_655 ? O5 W2 O6 156.1(3) . 12_656 ? O4 W2 O6 96.4(7) 11_556 12_656 ? O4 W2 O6 63.7(6) . 12_656 ? O3 W2 O6 96.5(6) 10_566 12_656 ? O3 W2 O6 63.9(5) 4_565 12_656 ? O6 W2 O6 47.8(7) 2_655 12_656 ? O5 W2 K1 83.2(6) . 2_655 ? O4 W2 K1 46.9(3) 11_556 2_655 ? O4 W2 K1 46.9(3) . 2_655 ? O3 W2 K1 136.2(3) 10_566 2_655 ? O3 W2 K1 136.2(3) 4_565 2_655 ? O6 W2 K1 95.4(4) 2_655 2_655 ? O6 W2 K1 95.4(4) 12_656 2_655 ? O5 W2 K1 87.3(6) . . ? O4 W2 K1 135.7(3) 11_556 . ? O4 W2 K1 135.7(3) . . ? O3 W2 K1 46.0(3) 10_566 . ? O3 W2 K1 46.0(3) 4_565 . ? O6 W2 K1 93.3(4) 2_655 . ? O6 W2 K1 93.3(4) 12_656 . ? K1 W2 K1 170.48(8) 2_655 . ? W2 O4 W1 136.9(8) . . ? W2 O4 K1 104.1(4) . 2_655 ? W1 O4 K1 106.2(4) . 2_655 ? O6 Si1 O6 180.000(2) 9_666 . ? O6 Si1 O6 109.6(5) 9_666 4_565 ? O6 Si1 O6 70.4(5) . 4_565 ? O6 Si1 O6 70.4(5) 9_666 12_656 ? O6 Si1 O6 109.6(5) . 12_656 ? O6 Si1 O6 180.000(2) 4_565 12_656 ? O6 Si1 O6 70.7(9) 9_666 3_665 ? O6 Si1 O6 109.3(9) . 3_665 ? O6 Si1 O6 70.4(5) 4_565 3_665 ? O6 Si1 O6 109.6(5) 12_656 3_665 ? O6 Si1 O6 109.6(5) 9_666 2_655 ? O6 Si1 O6 70.4(5) . 2_655 ? O6 Si1 O6 109.3(9) 4_565 2_655 ? O6 Si1 O6 70.7(9) 12_656 2_655 ? O6 Si1 O6 70.4(5) 3_665 2_655 ? O6 Si1 O6 70.4(5) 9_666 10_566 ? O6 Si1 O6 109.6(5) . 10_566 ? O6 Si1 O6 70.7(9) 4_565 10_566 ? O6 Si1 O6 109.3(9) 12_656 10_566 ? O6 Si1 O6 109.6(5) 3_665 10_566 ? O6 Si1 O6 180.000(2) 2_655 10_566 ? O6 Si1 O6 109.3(9) 9_666 11_556 ? O6 Si1 O6 70.7(9) . 11_556 ? O6 Si1 O6 109.6(5) 4_565 11_556 ? O6 Si1 O6 70.4(5) 12_656 11_556 ? O6 Si1 O6 180.0(6) 3_665 11_556 ? O6 Si1 O6 109.6(5) 2_655 11_556 ? O6 Si1 O6 70.4(5) 10_566 11_556 ? O1 K1 O1 138.1(4) 13_755 6_646 ? O1 K1 O10 72.9(3) 13_755 7_545 ? O1 K1 O10 72.9(3) 6_646 7_545 ? O1 K1 O7 96(2) 13_755 . ? O1 K1 O7 76(2) 6_646 . ? O10 K1 O7 112.9(7) 7_545 . ? O1 K1 O7 76(2) 13_755 11_556 ? O1 K1 O7 96(2) 6_646 11_556 ? O10 K1 O7 112.9(7) 7_545 11_556 ? O7 K1 O7 20(4) . 11_556 ? O1 K1 O4 80.0(4) 13_755 10_566 ? O1 K1 O4 132.5(4) 6_646 10_566 ? O10 K1 O4 105.4(5) 7_545 10_566 ? O7 K1 O4 138.2(12) . 10_566 ? O7 K1 O4 125.7(16) 11_556 10_566 ? O1 K1 O4 132.5(4) 13_755 4_565 ? O1 K1 O4 80.0(4) 6_646 4_565 ? O10 K1 O4 105.4(5) 7_545 4_565 ? O7 K1 O4 125.7(16) . 4_565 ? O7 K1 O4 138.2(12) 11_556 4_565 ? O4 K1 O4 54.0(6) 10_566 4_565 ? O1 K1 O3 135.3(3) 13_755 4_565 ? O1 K1 O3 83.2(3) 6_646 4_565 ? O10 K1 O3 151.1(3) 7_545 4_565 ? O7 K1 O3 75.6(11) . 4_565 ? O7 K1 O3 84.8(11) 11_556 4_565 ? O4 K1 O3 78.8(5) 10_566 4_565 ? O4 K1 O3 53.4(4) 4_565 4_565 ? O1 K1 O3 83.2(3) 13_755 10_566 ? O1 K1 O3 135.3(3) 6_646 10_566 ? O10 K1 O3 151.1(3) 7_545 10_566 ? O7 K1 O3 84.8(11) . 10_566 ? O7 K1 O3 75.6(11) 11_556 10_566 ? O4 K1 O3 53.4(4) 10_566 10_566 ? O4 K1 O3 78.8(5) 4_565 10_566 ? O3 K1 O3 52.7(5) 4_565 10_566 ? O1 K1 W2 103.6(3) 13_755 10_566 ? O1 K1 W2 103.6(3) 6_646 10_566 ? O10 K1 W2 96.6(4) 7_545 10_566 ? O7 K1 W2 148.6(9) . 10_566 ? O7 K1 W2 148.6(9) 11_556 10_566 ? O4 K1 W2 28.9(2) 10_566 10_566 ? O4 K1 W2 28.9(2) 4_565 10_566 ? O3 K1 W2 73.2(3) 4_565 10_566 ? O3 K1 W2 73.2(3) 10_566 10_566 ? O1 K1 Co2 103.6(3) 13_755 10_566 ? O1 K1 Co2 103.6(3) 6_646 10_566 ? O10 K1 Co2 96.6(4) 7_545 10_566 ? O7 K1 Co2 148.6(9) . 10_566 ? O7 K1 Co2 148.6(9) 11_556 10_566 ? O4 K1 Co2 28.9(2) 10_566 10_566 ? O4 K1 Co2 28.9(2) 4_565 10_566 ? O3 K1 Co2 73.2(3) 4_565 10_566 ? O3 K1 Co2 73.2(3) 10_566 10_566 ? W2 K1 Co2 0.00(2) 10_566 10_566 ? O1 K1 Co1 70.3(2) 13_755 10_566 ? O1 K1 Co1 151.2(2) 6_646 10_566 ? O10 K1 Co1 124.2(3) 7_545 10_566 ? O7 K1 Co1 111.0(14) . 10_566 ? O7 K1 Co1 97.3(15) 11_556 10_566 ? O4 K1 Co1 28.4(2) 10_566 10_566 ? O4 K1 Co1 73.2(4) 4_565 10_566 ? O3 K1 Co1 72.5(3) 4_565 10_566 ? O3 K1 Co1 28.6(2) 10_566 10_566 ? W2 K1 Co1 55.09(5) 10_566 10_566 ? Co2 K1 Co1 55.09(5) 10_566 10_566 ? W1 O2 Co1 138.4(10) . 4_565 ? W1 O2 W1 138.4(10) . 4_565 ? W1 O1 K1 157.1(5) . 13_766 ? W1 O3 Co2 136.1(8) . 2_655 ? W1 O3 W2 136.1(8) . 2_655 ? W1 O3 K1 103.9(4) . 2_655 ? Co2 O3 K1 106.2(4) 2_655 2_655 ? W2 O3 K1 106.2(4) 2_655 2_655 ? Si1 O6 Co2 120.8(7) . 10_566 ? Si1 O6 W2 120.8(7) . 10_566 ? Si1 O6 W1 121.4(7) . 9_666 ? Co2 O6 W1 95.9(5) 10_566 9_666 ? W2 O6 W1 95.9(5) 10_566 9_666 ? Si1 O6 Co1 121.4(7) . 9_666 ? Co2 O6 Co1 95.9(5) 10_566 9_666 ? W2 O6 Co1 95.9(5) 10_566 9_666 ? Si1 O6 Co1 120.8(7) . 10_566 ? Co2 O6 Co1 96.0(5) 10_566 10_566 ? W2 O6 Co1 96.0(5) 10_566 10_566 ? W1 O6 Co1 95.8(5) 9_666 10_566 ? Co1 O6 Co1 95.8(5) 9_666 10_566 ? Si1 O6 W1 120.8(7) . 10_566 ? Co2 O6 W1 96.0(5) 10_566 10_566 ? W2 O6 W1 96.0(5) 10_566 10_566 ? W1 O6 W1 95.8(5) 9_666 10_566 ? Co1 O6 W1 95.8(5) 9_666 10_566 ? O7 O7 K1 80(2) 11_556 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 W2 O4 W1 -155.4(12) . . . . ? O4 W2 O4 W1 105.3(9) 11_556 . . . ? O3 W2 O4 W1 25(2) 10_566 . . . ? O3 W2 O4 W1 -54.3(12) 4_565 . . . ? O6 W2 O4 W1 42.3(12) 2_655 . . . ? O6 W2 O4 W1 6.4(10) 12_656 . . . ? K1 W2 O4 W1 133.6(16) 2_655 . . . ? K1 W2 O4 W1 -59.2(16) . . . . ? O5 W2 O4 K1 71.0(7) . . . 2_655 ? O4 W2 O4 K1 -28.3(10) 11_556 . . 2_655 ? O3 W2 O4 K1 -108.8(12) 10_566 . . 2_655 ? O3 W2 O4 K1 172.1(7) 4_565 . . 2_655 ? O6 W2 O4 K1 -91.4(6) 2_655 . . 2_655 ? O6 W2 O4 K1 -127.3(8) 12_656 . . 2_655 ? K1 W2 O4 K1 167.18(13) . . . 2_655 ? O1 W1 O4 W2 154.4(12) . . . . ? O2 W1 O4 W2 53.5(13) . . . . ? O2 W1 O4 W2 -26(2) 2_655 . . . ? O3 W1 O4 W2 -105.1(13) . . . . ? O6 W1 O4 W2 -42.0(12) 9_666 . . . ? O6 W1 O4 W2 -6.4(10) 12_656 . . . ? K1 W1 O4 W2 -133.1(16) 2_655 . . . ? O1 W1 O4 K1 -72.6(7) . . . 2_655 ? O2 W1 O4 K1 -173.4(8) . . . 2_655 ? O2 W1 O4 K1 106.8(11) 2_655 . . 2_655 ? O3 W1 O4 K1 28.0(7) . . . 2_655 ? O6 W1 O4 K1 91.1(7) 9_666 . . 2_655 ? O6 W1 O4 K1 126.7(8) 12_656 . . 2_655 ? O1 W1 O2 Co1 -156.7(12) . . . 4_565 ? O2 W1 O2 Co1 103.6(9) 2_655 . . 4_565 ? O3 W1 O2 Co1 22(2) . . . 4_565 ? O4 W1 O2 Co1 -54.2(13) . . . 4_565 ? O6 W1 O2 Co1 41.2(13) 9_666 . . 4_565 ? O6 W1 O2 Co1 6.1(11) 12_656 . . 4_565 ? K1 W1 O2 Co1 -60.6(17) 2_655 . . 4_565 ? O1 W1 O2 W1 -156.7(12) . . . 4_565 ? O2 W1 O2 W1 103.6(9) 2_655 . . 4_565 ? O3 W1 O2 W1 22(2) . . . 4_565 ? O4 W1 O2 W1 -54.2(13) . . . 4_565 ? O6 W1 O2 W1 41.2(13) 9_666 . . 4_565 ? O6 W1 O2 W1 6.1(11) 12_656 . . 4_565 ? K1 W1 O2 W1 -60.6(17) 2_655 . . 4_565 ? O2 W1 O1 K1 -40.4(19) . . . 13_766 ? O2 W1 O1 K1 48.9(19) 2_655 . . 13_766 ? O3 W1 O1 K1 140.2(18) . . . 13_766 ? O4 W1 O1 K1 -131.3(18) . . . 13_766 ? O6 W1 O1 K1 92(2) 9_666 . . 13_766 ? O6 W1 O1 K1 -83(2) 12_656 . . 13_766 ? K1 W1 O1 K1 -174.2(19) 2_655 . . 13_766 ? O1 W1 O3 Co2 -152.7(11) . . . 2_655 ? O2 W1 O3 Co2 29(2) . . . 2_655 ? O2 W1 O3 Co2 -52.7(12) 2_655 . . 2_655 ? O4 W1 O3 Co2 105.2(12) . . . 2_655 ? O6 W1 O3 Co2 7.1(9) 9_666 . . 2_655 ? O6 W1 O3 Co2 42.8(11) 12_656 . . 2_655 ? K1 W1 O3 Co2 132.1(15) 2_655 . . 2_655 ? O1 W1 O3 W2 -152.7(11) . . . 2_655 ? O2 W1 O3 W2 29(2) . . . 2_655 ? O2 W1 O3 W2 -52.7(12) 2_655 . . 2_655 ? O4 W1 O3 W2 105.2(12) . . . 2_655 ? O6 W1 O3 W2 7.1(9) 9_666 . . 2_655 ? O6 W1 O3 W2 42.8(11) 12_656 . . 2_655 ? K1 W1 O3 W2 132.1(15) 2_655 . . 2_655 ? O1 W1 O3 K1 75.1(7) . . . 2_655 ? O2 W1 O3 K1 -103.2(12) . . . 2_655 ? O2 W1 O3 K1 175.2(7) 2_655 . . 2_655 ? O4 W1 O3 K1 -26.9(6) . . . 2_655 ? O6 W1 O3 K1 -125.0(7) 9_666 . . 2_655 ? O6 W1 O3 K1 -89.3(6) 12_656 . . 2_655 ? O6 Si1 O6 Co2 -120.3(11) 4_565 . . 10_566 ? O6 Si1 O6 Co2 59.7(11) 12_656 . . 10_566 ? O6 Si1 O6 Co2 179.8(10) 3_665 . . 10_566 ? O6 Si1 O6 Co2 119.8(11) 2_655 . . 10_566 ? O6 Si1 O6 Co2 -60.2(11) 10_566 . . 10_566 ? O6 Si1 O6 W2 -120.3(11) 4_565 . . 10_566 ? O6 Si1 O6 W2 59.7(11) 12_656 . . 10_566 ? O6 Si1 O6 W2 179.8(10) 3_665 . . 10_566 ? O6 Si1 O6 W2 119.8(11) 2_655 . . 10_566 ? O6 Si1 O6 W2 -60.2(11) 10_566 . . 10_566 ? O6 Si1 O6 W1 179.9(9) 12_656 . . 9_666 ? O6 Si1 O6 W1 -60.0(6) 3_665 . . 9_666 ? O6 Si1 O6 W1 -120.0(3) 2_655 . . 9_666 ? O6 Si1 O6 W1 60.0(3) 10_566 . . 9_666 ? O6 Si1 O6 W1 120.0(6) 11_556 . . 9_666 ? O6 Si1 O6 Co1 179.9(9) 12_656 . . 9_666 ? O6 Si1 O6 Co1 -60.0(6) 3_665 . . 9_666 ? O6 Si1 O6 Co1 -120.0(3) 2_655 . . 9_666 ? O6 Si1 O6 Co1 60.0(3) 10_566 . . 9_666 ? O6 Si1 O6 Co1 120.0(6) 11_556 . . 9_666 ? O6 Si1 O6 Co1 120.0(3) 4_565 . . 10_566 ? O6 Si1 O6 Co1 -60.0(3) 12_656 . . 10_566 ? O6 Si1 O6 Co1 60.0(6) 3_665 . . 10_566 ? O6 Si1 O6 Co1 -179.9(9) 10_566 . . 10_566 ? O6 Si1 O6 Co1 -120.0(6) 11_556 . . 10_566 ? O6 Si1 O6 W1 120.0(3) 4_565 . . 10_566 ? O6 Si1 O6 W1 -60.0(3) 12_656 . . 10_566 ? O6 Si1 O6 W1 60.0(6) 3_665 . . 10_566 ? O6 Si1 O6 W1 -179.9(9) 10_566 . . 10_566 ? O6 Si1 O6 W1 -120.0(6) 11_556 . . 10_566 ? O1 K1 O7 O7 20.6(2) 13_755 . . 11_556 ? O1 K1 O7 O7 158.9(3) 6_646 . . 11_556 ? O10 K1 O7 O7 94.4(9) 7_545 . . 11_556 ? O4 K1 O7 O7 -61(2) 10_566 . . 11_556 ? O4 K1 O7 O7 -134.3(12) 4_565 . . 11_556 ? O3 K1 O7 O7 -114.8(6) 4_565 . . 11_556 ? O3 K1 O7 O7 -62.0(4) 10_566 . . 11_556 ? W2 K1 O7 O7 -107(3) 10_566 . . 11_556 ? Co2 K1 O7 O7 -107(3) 10_566 . . 11_556 ? Co1 K1 O7 O7 -50.4(6) 10_566 . . 11_556 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.557 _refine_diff_density_min -3.960 _refine_diff_density_rms 0.368 #============================================================================# # Luis Cunha-Silva @ DQB/FCUP & REQUIMTE * 12/01/2012 * END # #============================================================================#