# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jeffery Tallon' _publ_contact_author_email J.TALLON@IRL.CRI.NZ _publ_section_title ; Synthesis and structure of Na+-intercalated WO3(4,4'-bipyridyl)0.5 ; loop_ _publ_author_name 'Jeffery Tallon' 'Matthew R. Fox' 'Graeme J. Gainsford' 'Geoffrey Jameson' 'John Kennedy' 'Andreas Markwitz' ; H.Martin ; 'Islah Udin' # Attachment 'W2O6Bipy_LT_Pbca.cif' data_w2o6bipy_lt_pbca _database_code_depnum_ccdc_archive 'CCDC 734223' #TrackingRef 'W2O6Bipy_LT_Pbca.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 N2 O6 W2' _chemical_formula_sum 'C10 H8 N2 O6 W2' _chemical_formula_weight 619.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 7.47709(13) _cell_length_b 7.38736(13) _cell_length_c 22.56247(41) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1246.26(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 4676 _cell_measurement_theta_min 14.21 _cell_measurement_theta_max 144.16 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 33.917 _exptl_absorpt_correction_T_min 0.379 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; data scaling includes absorption [ABSCOR, Higashi (1995)] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'confocal optics' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_device_details 'Curved image plate' _diffrn_measurement_method \w-scans _diffrn_measurement_details '108 images in steps of 5\%' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7368 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 7.11 _diffrn_reflns_theta_max 70.06 _reflns_number_total 1120 _reflns_number_gt 1070 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crystal Clear (Rigaku, 2005)' _computing_cell_refinement 'FS Process (Rigaku, 1998)' _computing_data_reduction 'FS Process (Rigaku, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL-6.10 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury (Macrae at al., 2006) and POV-RAY (Cason, 2003) ; _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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. There is clear evidence of substantial disorder on the equatorial oxygen atoms of the W-O layer. This disorder appears also to extend, but to a lesser extent to the W atoms. Disorder of the W atoms has not been modelled. The pyridyl ring is well ordered. Despite the small, although highly significant, difference in the a and b cell lengths, there is no evidence for significant twinning. A small number (20) of reflections with exceptionally poor agreement between Fcalc and Fobs were eliminated from refinement, possibly because the small crystal was mounted against a 0.15 mm glass fibre. ; _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^)+(0.0366P)^2^+11.4191P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00011(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1120 _refine_ls_number_parameters 111 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.52162(5) 0.05180(5) 0.263764(12) 0.0087(2) Uani 1 1 d . . . N1 N 0.5184(9) 0.0384(9) 0.1567(3) 0.0165(11) Uani 1 1 d U . . O3 O 0.5106(6) 0.0548(7) 0.3390(3) 0.0107(12) Uani 1 1 d U . . C2 C 0.6240(11) -0.0743(9) 0.1278(3) 0.0159(11) Uani 1 1 d U . . H2 H 0.7039 -0.1443 0.1495 0.019 Uiso 1 1 calc R . . C3 C 0.4043(10) 0.1413(10) 0.1243(3) 0.0162(11) Uani 1 1 d U . . H3 H 0.3300 0.2226 0.1439 0.019 Uiso 1 1 calc R . . C4 C 0.6218(11) -0.0934(10) 0.0672(3) 0.0167(11) Uani 1 1 d U . . H4 H 0.7004 -0.1743 0.0493 0.020 Uiso 1 1 calc R . . C5 C 0.5046(10) 0.0056(14) 0.0324(3) 0.0160(11) Uani 1 1 d U . . C6 C 0.3945(10) 0.1299(10) 0.0632(3) 0.0165(11) Uani 1 1 d U . . H6 H 0.3156 0.2037 0.0425 0.020 Uiso 1 1 calc R . . O1B O 0.458(2) -0.1977(17) 0.2514(5) 0.013(2) Uani 0.471(17) 1 d PU . 1 O2B O 0.7589(17) 0.006(3) 0.2522(4) 0.0117(19) Uani 0.471(17) 1 d PU . 1 O1A O 0.535(2) -0.2034(16) 0.2522(5) 0.0137(19) Uani 0.529(17) 1 d PU . 2 O2A O 0.7595(15) 0.085(2) 0.2518(4) 0.0123(19) Uani 0.529(17) 1 d PU . 2 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 0.0063(3) 0.0104(3) 0.0094(3) -0.00004(9) -0.00020(10) 0.00003(12) N1 0.0178(19) 0.0169(18) 0.0149(18) -0.0006(14) 0.0009(15) 0.0000(15) O3 0.0100(14) 0.0105(14) 0.0116(14) 0.0003(8) -0.0005(8) -0.0001(8) C2 0.0161(19) 0.0162(18) 0.0155(17) 0.0009(15) 0.0008(16) -0.0004(16) C3 0.0170(19) 0.0162(18) 0.0154(17) 0.0006(15) -0.0007(16) 0.0008(17) C4 0.0161(19) 0.0178(18) 0.0162(17) 0.0003(15) 0.0015(16) 0.0003(16) C5 0.0158(19) 0.0169(18) 0.0152(18) 0.0000(16) 0.0001(16) -0.0001(16) C6 0.0164(19) 0.0172(18) 0.0159(17) 0.0008(15) -0.0010(16) 0.0012(16) O1B 0.013(3) 0.015(3) 0.012(2) 0.002(2) 0.000(2) 0.000(2) O2B 0.014(3) 0.011(3) 0.010(2) -0.001(2) 0.001(2) 0.000(2) O1A 0.013(3) 0.016(3) 0.012(2) 0.002(2) -0.001(2) 0.001(2) O2A 0.015(3) 0.012(3) 0.010(2) 0.001(2) 0.000(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O3 1.700(6) . ? W1 O2A 1.815(11) . ? W1 O2B 1.825(13) . ? W1 O1A 1.892(12) 3_655 ? W1 O1B 1.888(13) 3_655 ? W1 O1A 1.906(12) . ? W1 O1B 1.924(13) . ? W1 O2A 2.006(11) 6_556 ? W1 O2B 2.025(13) 6_556 ? W1 N1 2.418(8) . ? N1 C2 1.320(10) . ? N1 C3 1.357(10) . ? C2 C4 1.375(9) . ? C3 C6 1.382(9) . ? C4 C5 1.386(11) . ? C5 C6 1.417(11) . ? C5 C5 1.464(15) 5_655 ? O1B W1 1.888(13) 3_645 ? O2B W1 2.025(13) 6_656 ? O1A W1 1.892(12) 3_645 ? O2A W1 2.006(11) 6_656 ? 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 O3 W1 O2A 101.2(3) . . ? O3 W1 O2B 101.1(3) . . ? O2A W1 O2B 18.4(5) . . ? O3 W1 O1A 99.6(4) . 3_655 ? O2A W1 O1A 93.6(5) . 3_655 ? O2B W1 O1A 111.6(6) . 3_655 ? O3 W1 O1B 99.9(4) . 3_655 ? O2A W1 O1B 76.3(5) . 3_655 ? O2B W1 O1B 94.4(6) . 3_655 ? O1A W1 O1B 17.6(5) 3_655 3_655 ? O3 W1 O1A 98.8(4) . . ? O2A W1 O1A 93.5(5) . . ? O2B W1 O1A 75.3(6) . . ? O1A W1 O1A 158.63(7) 3_655 . ? O1B W1 O1A 160.1(6) 3_655 . ? O3 W1 O1B 98.4(4) . . ? O2A W1 O1B 110.4(5) . . ? O2B W1 O1B 92.4(6) . . ? O1A W1 O1B 146.4(5) 3_655 . ? O1B W1 O1B 158.85(6) 3_655 . ? O1A W1 O1B 17.3(5) . . ? O3 W1 O2A 97.2(3) . 6_556 ? O2A W1 O2A 156.2(6) . 6_556 ? O2B W1 O2A 161.3(5) . 6_556 ? O1A W1 O2A 68.4(8) 3_655 6_556 ? O1B W1 O2A 85.8(8) 3_655 6_556 ? O1A W1 O2A 98.5(8) . 6_556 ? O1B W1 O2A 81.4(8) . 6_556 ? O3 W1 O2B 97.6(3) . 6_556 ? O2A W1 O2B 161.1(5) . 6_556 ? O2B W1 O2B 152.5(8) . 6_556 ? O1A W1 O2B 84.7(8) 3_655 6_556 ? O1B W1 O2B 102.0(9) 3_655 6_556 ? O1A W1 O2B 82.1(8) . 6_556 ? O1B W1 O2B 64.9(9) . 6_556 ? O2A W1 O2B 16.6(5) 6_556 6_556 ? O3 W1 N1 176.3(2) . . ? O2A W1 N1 82.4(3) . . ? O2B W1 N1 81.9(3) . . ? O1A W1 N1 81.2(4) 3_655 . ? O1B W1 N1 82.0(4) 3_655 . ? O1A W1 N1 79.8(4) . . ? O1B W1 N1 79.2(4) . . ? O2A W1 N1 79.6(3) 6_556 . ? O2B W1 N1 78.8(3) 6_556 . ? C2 N1 C3 117.7(7) . . ? C2 N1 W1 120.9(5) . . ? C3 N1 W1 121.4(5) . . ? N1 C2 C4 123.3(7) . . ? N1 C3 C6 122.4(7) . . ? C2 C4 C5 121.2(7) . . ? C4 C5 C6 115.5(7) . . ? C4 C5 C5 124.5(10) . 5_655 ? C6 C5 C5 120.0(9) . 5_655 ? C3 C6 C5 119.9(7) . . ? W1 O1B W1 161.0(10) 3_645 . ? W1 O2B W1 159.7(11) . 6_656 ? W1 O1A W1 163.7(9) 3_645 . ? W1 O2A W1 165.2(10) . 6_656 ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 70.06 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 3.860 _refine_diff_density_min -2.370 _refine_diff_density_rms 0.344 # Attachment 'W2O6Bipy_Na2LT_Pbca.cif' data_w2o6bipy_na2lt_pbca _database_code_depnum_ccdc_archive 'CCDC 734224' #TrackingRef 'W2O6Bipy_Na2LT_Pbca.cif' _audit_update_record ; 2009-05-19 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C10 H8 N20) Na0.25 (O6 W2)' _chemical_formula_sum 'C10 H8 N2 Na0.25 O6 W2' _chemical_formula_weight 625.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 7.4683(3) _cell_length_b 7.3910(3) _cell_length_c 22.5781(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1246.27(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(5) _cell_measurement_reflns_used 1187 _cell_measurement_theta_min 17.33 _cell_measurement_theta_max 143.02 # .... size to be checked _exptl_crystal_description plate _exptl_crystal_colour yellow-green _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1123 _exptl_absorpt_coefficient_mu 34.008 _exptl_absorpt_correction_T_min 0.008 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; data scaling includes absorption [ABSCOR, Higashi (1995)] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(5) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'confocal optics' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_device_details 'Curved image plate' _diffrn_measurement_method \w-scans _diffrn_measurement_details '100 images in steps of 5\%' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6727 _diffrn_reflns_av_R_equivalents 0.0936 _diffrn_reflns_av_sigmaI/netI 0.0790 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 7.11 _diffrn_reflns_theta_max 69.93 _reflns_number_total 1125 _reflns_number_gt 1015 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crystal Clear (Rigaku, 2005)' _computing_cell_refinement 'FS Process (Rigaku, 1998)' _computing_data_reduction 'FS Process (Rigaku, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL-6.10 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury (Macrae at al., 2006)' and POV-RAY (Cason, 2003) ; _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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. There is clear evidence of substantial disorder on the equatorial oxygen atoms of the W-O layer. This disorder appears also to extend, but to a lesser extent to the W atoms. Disorder of the W atoms has not been modelled. The pyridyl ring is well ordered. Despite the small, although highly significant, difference in the a and b cell lengths, there is no evidence for significant twinning. A small number (31) of reflections with exceptionally poor agreement between Fcalc and Fobs were eliminated from refinement, possibly because the small crystal was mounted against a 0.15 mm glass fibre, but also because of instabilities in the low temperature device. After sodium implantation, crystal quality was noticeably deteriorated and more highly mosaic. A sodium ion is present in low occupancy (0.125), in part because of disorder across a centre of inversion. It sits just off the axial W-O3 axis in a small cavity bounded by the O3 and the 4,4'-bipyridyl groups. ; _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^)+(0.0000P)^2^+146.9178P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00008(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1125 _refine_ls_number_parameters 115 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1279 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 0.865 _refine_ls_restrained_S_all 0.820 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 0.51977(8) 1.04669(11) 0.26376(2) 0.0146(3) Uani 1 1 d . . . N1 N 0.5138(15) 1.0339(18) 0.1567(5) 0.0188(16) Uani 1 1 d U . . O3 O 0.5089(11) 1.0501(14) 0.3396(4) 0.014(2) Uani 1 1 d U . . C2 C 0.6251(19) 0.922(2) 0.1280(6) 0.0196(17) Uani 1 1 d U . . H2 H 0.7060 0.8532 0.1498 0.024 Uiso 1 1 calc R . . C3 C 0.4034(18) 1.142(2) 0.1250(6) 0.0195(16) Uani 1 1 d U . . H3 H 0.3334 1.2277 0.1444 0.023 Uiso 1 1 calc R . . C4 C 0.6234(19) 0.905(2) 0.0665(6) 0.0201(17) Uani 1 1 d U . . H4 H 0.7019 0.8254 0.0479 0.024 Uiso 1 1 calc R . . C5 C 0.5027(18) 1.008(2) 0.0326(6) 0.0195(17) Uani 1 1 d U . . C6 C 0.3941(18) 1.126(2) 0.0636(6) 0.0199(16) Uani 1 1 d U . . H6 H 0.3125 1.1973 0.0429 0.024 Uiso 1 1 calc R . . O1A O 0.461(4) 0.783(3) 0.2523(8) 0.012(3) Uani 0.48(3) 1 d PU . 1 O2A O 0.760(3) 1.002(4) 0.2516(10) 0.024(3) Uani 0.48(3) 1 d PU . 1 O1B O 0.539(3) 0.778(3) 0.2517(8) 0.011(3) Uani 0.52(3) 1 d PU . 2 O2B O 0.759(3) 1.076(4) 0.2513(9) 0.024(3) Uani 0.52(3) 1 d PU . 2 Na1 Na 0.50(2) 1.03(2) 0.473(7) 0.18(7) Uiso 0.13 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 0.0157(4) 0.0168(5) 0.0114(4) -0.0010(2) -0.0002(2) 0.0036(3) N1 0.019(2) 0.019(2) 0.018(2) -0.0002(19) 0.0001(18) -0.0003(18) O3 0.015(2) 0.014(2) 0.015(2) 0.0001(15) -0.0003(15) -0.0003(15) C2 0.020(2) 0.019(2) 0.019(2) -0.0001(19) 0.0003(18) 0.0003(19) C3 0.020(2) 0.019(2) 0.019(2) -0.0006(19) 0.0002(18) 0.0000(19) C4 0.020(2) 0.020(2) 0.020(2) 0.0000(19) 0.0004(19) 0.0003(19) C5 0.020(2) 0.019(2) 0.019(2) -0.0002(19) 0.0002(19) 0.0000(19) C6 0.020(2) 0.020(2) 0.019(2) -0.0003(19) -0.0002(18) 0.0002(19) O1A 0.011(4) 0.011(3) 0.012(3) 0.003(2) 0.000(2) -0.001(2) O2A 0.025(4) 0.024(4) 0.023(4) 0.000(2) -0.001(2) 0.000(2) O1B 0.011(4) 0.011(3) 0.012(3) 0.003(2) 0.000(2) 0.001(2) O2B 0.024(4) 0.025(4) 0.023(4) 0.000(2) -0.001(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O3 1.715(9) . ? W1 O1A 1.79(2) 3_655 ? W1 O1B 1.80(2) 3_655 ? W1 O2B 1.82(2) . ? W1 O2A 1.85(3) . ? W1 O2B 1.99(2) 6_556 ? W1 O2A 2.00(3) 6_556 ? W1 O1B 2.01(2) . ? W1 O1A 2.01(2) . ? W1 N1 2.419(12) . ? N1 C2 1.340(18) . ? N1 C3 1.353(18) . ? O3 Na1 3.02(17) . ? C2 C4 1.395(19) . ? C3 C6 1.393(18) . ? C4 C5 1.41(2) . ? C4 Na1 3.07(17) 3_645 ? C4 Na1 3.10(18) 6_656 ? C5 C6 1.38(2) . ? C5 C5 1.48(3) 5_675 ? C6 Na1 3.13(17) 6_556 ? O1A W1 1.79(2) 3_645 ? O2A W1 2.00(3) 6_656 ? O1B W1 1.80(2) 3_645 ? O2B W1 1.99(2) 6_656 ? Na1 Na1 1.3(3) 5_676 ? Na1 C4 3.07(17) 3_655 ? Na1 C4 3.10(18) 6_556 ? Na1 C6 3.13(17) 6_656 ? 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 O3 W1 O1A 101.0(7) . 3_655 ? O3 W1 O1B 99.7(6) . 3_655 ? O1A W1 O1B 18.8(7) 3_655 3_655 ? O3 W1 O2B 101.4(7) . . ? O1A W1 O2B 76.9(9) 3_655 . ? O1B W1 O2B 95.6(9) 3_655 . ? O3 W1 O2A 101.4(7) . . ? O1A W1 O2A 93.8(10) 3_655 . ? O1B W1 O2A 112.2(10) 3_655 . ? O2B W1 O2A 17.1(10) . . ? O3 W1 O2B 97.1(7) . 6_556 ? O1A W1 O2B 86.6(14) 3_655 6_556 ? O1B W1 O2B 68.0(14) 3_655 6_556 ? O2B W1 O2B 157.2(10) . 6_556 ? O2A W1 O2B 161.1(12) . 6_556 ? O3 W1 O2A 97.5(7) . 6_556 ? O1A W1 O2A 101.9(15) 3_655 6_556 ? O1B W1 O2A 83.6(14) 3_655 6_556 ? O2B W1 O2A 160.9(11) . 6_556 ? O2A W1 O2A 152.7(13) . 6_556 ? O2B W1 O2A 15.7(9) 6_556 6_556 ? O3 W1 O1B 98.8(6) . . ? O1A W1 O1B 158.6(8) 3_655 . ? O1B W1 O1B 158.45(14) 3_655 . ? O2B W1 O1B 91.5(9) . . ? O2A W1 O1B 74.6(9) . . ? O2B W1 O1B 98.8(13) 6_556 . ? O2A W1 O1B 83.2(14) 6_556 . ? O3 W1 O1A 97.6(6) . . ? O1A W1 O1A 159.35(10) 3_655 . ? O1B W1 O1A 147.2(7) 3_655 . ? O2B W1 O1A 108.0(9) . . ? O2A W1 O1A 91.2(10) . . ? O2B W1 O1A 82.4(14) 6_556 . ? O2A W1 O1A 66.7(14) 6_556 . ? O1B W1 O1A 16.7(6) . . ? O3 W1 N1 176.0(4) . . ? O1A W1 N1 80.6(7) 3_655 . ? O1B W1 N1 80.7(6) 3_655 . ? O2B W1 N1 82.5(7) . . ? O2A W1 N1 82.1(7) . . ? O2B W1 N1 79.3(7) 6_556 . ? O2A W1 N1 78.6(7) 6_556 . ? O1B W1 N1 80.1(6) . . ? O1A W1 N1 80.2(6) . . ? C2 N1 C3 119.2(13) . . ? C2 N1 W1 119.7(9) . . ? C3 N1 W1 121.1(9) . . ? W1 O3 Na1 176(4) . . ? N1 C2 C4 122.1(13) . . ? N1 C3 C6 120.5(13) . . ? C2 C4 C5 119.9(13) . . ? C2 C4 Na1 112(3) . 3_645 ? C5 C4 Na1 98(3) . 3_645 ? C2 C4 Na1 105(3) . 6_656 ? C5 C4 Na1 105(4) . 6_656 ? C6 C5 C4 116.2(13) . . ? C6 C5 C5 122.8(17) . 5_675 ? C4 C5 C5 121.0(16) . 5_675 ? C5 C6 C3 121.9(14) . . ? C5 C6 Na1 106(3) . 6_556 ? C3 C6 Na1 109(3) . 6_556 ? W1 O1A W1 162.1(16) 3_645 . ? W1 O2A W1 160.0(18) . 6_656 ? W1 O1B W1 161.5(15) 3_645 . ? W1 O2B W1 167.0(17) . 6_656 ? O3 Na1 C4 71(3) . 3_655 ? O3 Na1 C4 75(4) . 6_556 ? C4 Na1 C4 85(4) 3_655 6_556 ? O3 Na1 C6 73(4) . 6_656 ? C4 Na1 C6 90(4) 3_655 6_656 ? C4 Na1 C6 148(6) 6_556 6_656 ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 69.93 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 3.252 _refine_diff_density_min -3.223 _refine_diff_density_rms 0.399 # Attachment 'W2O6Bipy_Na4RT_Pbca.cif' data_w2o6bipy_na4rt_pbca _database_code_depnum_ccdc_archive 'CCDC 734225' #TrackingRef 'W2O6Bipy_Na4RT_Pbca.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C10 H8 N2) 0.13(Na2) 2(O3 W)' _chemical_formula_sum 'C10 H8 N2 Na0.26 O6 W2' _chemical_formula_weight 625.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 7.48501(14) _cell_length_b 7.40943(15) _cell_length_c 22.6257(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1254.81(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8286 _cell_measurement_theta_min 14.2 _cell_measurement_theta_max 144.1 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 3.313 _exptl_crystal_F_000 1123 _exptl_absorpt_coefficient_mu 33.777 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1313 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; data scaling includes absorption [ABSCOR, Higashi (1995)] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'confocal optics' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_device_details 'Curved image plate' _diffrn_measurement_method \w-scans _diffrn_measurement_details '101 images in steps of 5\%' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7095 _diffrn_reflns_av_R_equivalents 0.1264 _diffrn_reflns_av_sigmaI/netI 0.0972 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 7.09 _diffrn_reflns_theta_max 72.03 _reflns_number_total 1192 _reflns_number_gt 1018 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crystal Clear (Rigaku, 2005)' _computing_cell_refinement 'FS Process (Rigaku, 1998)' _computing_data_reduction 'FS Process (Rigaku, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury (Macrae at al., 2006)' and POV-RAY (Cason, 2003) ; _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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. Restraints were placed on the anisotropic atomic displacement parameters of all C, N and O atoms (e.g. ISOR 0.005 $C, $N, $O), as is generally good practice for structures containing heavy metal ions such as tungsten, especially with weak data from very small crystals as is the case here, and for the situation of disordered atoms separated by distances similar to the resolution of the data, as is the case here for several oxygen sites (e.g. SIMU 0.003 1.2 $O). Despite poor merging statistics for orthorhombic mmm symmetry and a number (19) of reflections that merged very poorly, the final values for R1(observed data) and wR2 are satisfactory and comparable to other data sets with and without sodium implantation. There is clear evidence of substantial disorder on the equatorial oxygen atoms of the W-O layer. This disorder appears also to extend, but to a lesser extent to the W atoms. Disorder of the W atoms has not been modelled. The pyridyl ring is well ordered. Despite the small, although highly significant, difference in the a and b cell lengths, there is no evidence for significant twinning. A small number (16) of reflections with exceptionally poor agreement between Fcalc and Fobs were eliminated from refinement, possibly because the small crystal was mounted against a 0.15 mm glass fibre, but also because of instabilities in the low temperature device. After sodium implantation (4% w/w), crystal quality was noticeably deteriorated and more highly mosaic. The substantial number (22) of violations of systematic absences for space group Pbca is attributed to partial overlap of reflections. A sodium ion is present in low occupancy (0.125), in part because of disorder across a centre of inversion. It sits just off the axial W-O3 axis in a small cavity bounded by the O3 and the 4,4'-bipyridyl groups. ; _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^)+(0.0654P)^2^+1.8147P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00011(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1192 _refine_ls_number_parameters 115 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1221 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.52026(7) 0.04605(6) 0.263542(15) 0.0158(3) Uani 1 1 d U . . O1A O 0.538(3) -0.214(2) 0.2523(7) 0.018(3) Uani 0.52(2) 1 d PU . 1 O2A O 0.7601(19) 0.076(3) 0.2508(5) 0.019(3) Uani 0.52(2) 1 d PU . 1 O3 O 0.5110(7) 0.0484(7) 0.3383(4) 0.0174(13) Uani 1 1 d U . . O1B O 0.463(3) -0.211(2) 0.2532(7) 0.016(3) Uani 0.48(2) 1 d PU . 2 O2B O 0.759(2) 0.005(4) 0.2522(5) 0.019(3) Uani 0.48(2) 1 d PU . 2 N1 N 0.5157(10) 0.0361(11) 0.1550(5) 0.0299(14) Uani 1 1 d U . 2 C1 C 0.6209(13) -0.0979(10) 0.0668(3) 0.0298(13) Uani 1 1 d U . 2 H1 H 0.6972 -0.1803 0.0488 0.036 Uiso 1 1 calc R . 2 C2 C 0.4025(12) 0.1356(11) 0.1242(3) 0.0292(13) Uani 1 1 d U . 2 H2 H 0.3271 0.2145 0.1442 0.035 Uiso 1 1 calc R . 2 C3 C 0.3924(12) 0.1265(10) 0.0640(3) 0.0298(13) Uani 1 1 d U . 2 H3 H 0.3117 0.1996 0.0439 0.036 Uiso 1 1 calc R . 2 C4 C 0.5038(13) 0.006(2) 0.0318(5) 0.0297(14) Uani 1 1 d U . 2 C6 C 0.6233(13) -0.0789(11) 0.1272(3) 0.0297(13) Uani 1 1 d U . . H6 H 0.7024 -0.1484 0.1493 0.036 Uiso 1 1 calc R . 2 Na1 Na 0.515(9) -0.969(13) 0.469(6) 0.14(3) Uiso 0.13 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 0.0125(4) 0.0173(4) 0.0175(4) -0.00049(12) -0.00012(12) 0.00013(14) O1A 0.017(5) 0.014(4) 0.022(3) 0.001(3) 0.000(4) 0.001(4) O2A 0.017(4) 0.017(5) 0.022(3) 0.007(3) 0.001(3) -0.001(4) O3 0.014(2) 0.017(2) 0.022(2) -0.0007(18) -0.0009(17) 0.0021(15) O1B 0.015(5) 0.012(4) 0.021(3) -0.003(3) 0.001(4) 0.001(4) O2B 0.017(4) 0.018(5) 0.022(3) 0.003(3) 0.000(3) 0.000(4) N1 0.030(3) 0.031(3) 0.029(3) -0.004(2) 0.002(2) 0.003(2) C1 0.028(3) 0.032(3) 0.030(3) -0.002(2) 0.000(2) 0.008(2) C2 0.029(3) 0.030(3) 0.029(3) -0.004(2) 0.000(2) 0.005(2) C3 0.028(3) 0.030(3) 0.031(3) -0.003(2) 0.000(2) 0.007(2) C4 0.028(3) 0.030(3) 0.031(3) -0.002(3) 0.000(2) 0.007(2) C6 0.028(3) 0.031(3) 0.030(3) -0.003(2) 0.001(2) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O3 1.692(8) . ? W1 O2B 1.829(16) . ? W1 O2A 1.832(14) . ? W1 O1B 1.848(16) 3_655 ? W1 O1A 1.866(16) 3_655 ? W1 O1A 1.947(16) . ? W1 O1B 1.963(17) . ? W1 O2A 1.987(15) 6_556 ? W1 O2B 2.013(16) 6_556 ? W1 N1 2.456(12) . ? O1A W1 1.866(16) 3_645 ? O2A W1 1.987(14) 6_656 ? O3 Na1 2.97(14) 1_565 ? O1B W1 1.848(16) 3_645 ? O2B W1 2.013(16) 6_656 ? N1 C2 1.323(12) . ? N1 C6 1.330(12) . ? C1 C6 1.375(10) . ? C1 C4 1.412(15) . ? C1 Na1 3.04(9) 3_655 ? C1 H1 0.9300 . ? C2 C3 1.366(11) . ? C2 H2 0.9300 . ? C3 C4 1.420(15) . ? C3 Na1 3.01(7) 6_566 ? C3 H3 0.9300 . ? C4 C4 1.44(2) 5_655 ? C6 H6 0.9300 . ? Na1 Na1 1.5(3) 5_636 ? Na1 O3 2.97(14) 1_545 ? Na1 C3 3.01(7) 6_646 ? Na1 C1 3.04(9) 3_645 ? 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 O3 W1 O2B 100.5(4) . . ? O3 W1 O2A 101.3(4) . . ? O2B W1 O2A 16.7(8) . . ? O3 W1 O1B 101.4(5) . 3_655 ? O2B W1 O1B 93.8(8) . 3_655 ? O2A W1 O1B 77.3(7) . 3_655 ? O3 W1 O1A 100.0(5) . 3_655 ? O2B W1 O1A 111.1(8) . 3_655 ? O2A W1 O1A 94.7(7) . 3_655 ? O1B W1 O1A 17.5(7) 3_655 3_655 ? O3 W1 O1A 98.2(5) . . ? O2B W1 O1A 75.5(8) . . ? O2A W1 O1A 92.0(7) . . ? O1B W1 O1A 159.1(8) 3_655 . ? O1A W1 O1A 159.00(10) 3_655 . ? O3 W1 O1B 96.9(5) . . ? O2B W1 O1B 92.1(8) . . ? O2A W1 O1B 108.4(7) . . ? O1B W1 O1B 159.41(6) 3_655 . ? O1A W1 O1B 148.1(7) 3_655 . ? O1A W1 O1B 16.6(6) . . ? O3 W1 O2A 97.0(4) . 6_556 ? O2B W1 O2A 162.2(6) . 6_556 ? O2A W1 O2A 157.1(8) . 6_556 ? O1B W1 O2A 85.7(11) 3_655 6_556 ? O1A W1 O2A 68.4(11) 3_655 6_556 ? O1A W1 O2A 99.0(10) . 6_556 ? O1B W1 O2A 82.8(11) . 6_556 ? O3 W1 O2B 97.9(4) . 6_556 ? O2B W1 O2B 154.0(11) . 6_556 ? O2A W1 O2B 160.7(6) . 6_556 ? O1B W1 O2B 100.4(11) 3_655 6_556 ? O1A W1 O2B 83.3(11) 3_655 6_556 ? O1A W1 O2B 83.8(11) . 6_556 ? O1B W1 O2B 67.5(11) . 6_556 ? O2A W1 O2B 15.2(8) 6_556 6_556 ? O3 W1 N1 176.7(3) . . ? O2B W1 N1 82.4(4) . . ? O2A W1 N1 82.0(4) . . ? O1B W1 N1 79.9(5) 3_655 . ? O1A W1 N1 80.4(5) 3_655 . ? O1A W1 N1 80.9(5) . . ? O1B W1 N1 81.3(5) . . ? O2A W1 N1 80.0(4) 6_556 . ? O2B W1 N1 78.8(4) 6_556 . ? W1 O1A W1 162.2(11) 3_645 . ? W1 O2A W1 166.5(14) . 6_656 ? W1 O3 Na1 175.7(17) . 1_565 ? W1 O1B W1 162.6(12) 3_645 . ? W1 O2B W1 161.5(15) . 6_656 ? C2 N1 C6 119.7(10) . . ? C2 N1 W1 121.3(7) . . ? C6 N1 W1 118.9(7) . . ? C6 C1 C4 120.6(9) . . ? C6 C1 Na1 111(3) . 3_655 ? C4 C1 Na1 98(2) . 3_655 ? C6 C1 H1 119.7 . . ? C4 C1 H1 119.7 . . ? Na1 C1 H1 59.6 3_655 . ? N1 C2 C3 122.3(9) . . ? N1 C2 H2 118.9 . . ? C3 C2 H2 118.9 . . ? C2 C3 C4 120.7(9) . . ? C2 C3 Na1 108(3) . 6_566 ? C4 C3 Na1 106(2) . 6_566 ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? Na1 C3 H3 53.5 6_566 . ? C1 C4 C3 114.8(10) . . ? C1 C4 C4 123.2(14) . 5_655 ? C3 C4 C4 122.0(14) . 5_655 ? N1 C6 C1 121.9(9) . . ? N1 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? Na1 Na1 O3 162(9) 5_636 1_545 ? Na1 Na1 C3 116(7) 5_636 6_646 ? O3 Na1 C3 75(3) 1_545 6_646 ? Na1 Na1 C1 119(9) 5_636 3_645 ? O3 Na1 C1 72(3) 1_545 3_645 ? C3 Na1 C1 92(2) 6_646 3_645 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 72.03 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 4.473 _refine_diff_density_min -2.192 _refine_diff_density_rms 0.508