Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 1145 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; New Metathesis Routes to layered dichalcogenides: synthesis, crystal growth and structure of NayNbX2(y=0.5, X=S, Se). ; _publ_contact_author ' D.H. Gregory' _publ_contact_author_email 'duncan.gregory@nottingham.ac.uk' _publ_contact_author_address ; School of Chemistry University of Nottingham University Park Nottingham NG7 2RD ; loop_ _publ_author_name 'Pamela A. Salyer' 'Marten G. Barker' 'Alexander J. Blake' 'Duncan H. Gregory' 'David P. Weston' 'Claire Wilson' data_nanbse _database_code_CSD 195103 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'sodium niobium diselenide' _chemical_melting_point ? _chemical_formula_moiety 'Na0.50 Nb Se2' _chemical_formula_sum 'Na0.50 Nb Se2' _chemical_formula_weight 262.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3)/mmc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z' '-x+y, -x, z' 'x-y, x, z+1/2' 'y, -x+y, z+1/2' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' '-y, -x, -z+1/2' 'x, x-y, -z+1/2' '-x+y, y, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, -x, -z-1/2' '-y, x-y, -z-1/2' '-x+y, y, z' 'x, x-y, z' '-y, -x, z' 'y, x, z-1/2' '-x, -x+y, z-1/2' 'x-y, -y, z-1/2' _cell_length_a 3.4762(7) _cell_length_b 3.4762(7) _cell_length_c 15.342(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 160.55(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 383 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 28.05 _exptl_crystal_description plate _exptl_crystal_colour metallic _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 5.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 229 _exptl_absorpt_coefficient_mu 26.169 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.617 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS v2.03(2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 702 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 28.29 _reflns_number_total 100 _reflns_number_gt 91 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOMS 4.1 (Dowty, 1998)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 100 _refine_ls_number_parameters 10 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0230 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0487 _refine_ls_wR_factor_gt 0.0474 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _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 Nb1 Nb 0.3333 0.6667 0.2500 0.0029(3) Uani 1 12 d S . . Se1 Se 0.0000 0.0000 0.35817(5) 0.0032(3) Uani 1 6 d S . . Na1 Na 0.6667 0.3333 0.5009(8) 0.016(5) Uani 0.249(14) 6 d SP . . 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 Nb1 0.0023(4) 0.0023(4) 0.0042(5) 0.000 0.000 0.0011(2) Se1 0.0023(4) 0.0023(4) 0.0050(5) 0.000 0.000 0.00116(18) Na1 0.022(7) 0.022(7) 0.002(7) 0.000 0.000 0.011(3) _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 Nb1 Nb1 3.4762(7) 1_445 ? Nb1 Se1 2.6043(6) 14_556 ? Nb1 Se1 2.6043(6) 1_665 ? Nb1 Se1 2.6043(6) 14_566 ? Nb1 Se1 2.6043(6) 1_565 ? Nb1 Se1 2.6043(6) 14_666 ? Nb1 Se1 2.6043(6) . ? Se1 Nb1 2.6043(6) 1_445 ? Se1 Nb1 2.6043(6) 1_545 ? Se1 Na1 2.950(10) 13_666 ? Se1 Na1 2.950(10) 13_656 ? Se1 Na1 2.950(10) 13_556 ? Se1 Na1 2.971(10) . ? Se1 Na1 2.971(10) 1_455 ? Se1 Na1 2.971(10) 1_445 ? Na1 Se1 2.950(10) 13_666 ? Na1 Se1 2.950(10) 13_656 ? Na1 Se1 2.950(10) 13_556 ? Na1 Se1 2.971(10) 1_655 ? Na1 Se1 2.971(10) 1_665 ? Se1 Se1 3.3192(16) 14_556 ? Na1 Nb1 3.821(13) 13_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 Se1 Nb1 Se1 134.672(10) 14_556 1_665 ? Se1 Nb1 Se1 83.73(2) 14_556 14_566 ? Se1 Nb1 Se1 134.672(10) 1_665 14_566 ? Se1 Nb1 Se1 134.672(10) 14_556 1_565 ? Se1 Nb1 Se1 83.73(2) 1_665 1_565 ? Se1 Nb1 Se1 79.18(3) 14_566 1_565 ? Se1 Nb1 Se1 83.73(2) 14_556 14_666 ? Se1 Nb1 Se1 79.18(3) 1_665 14_666 ? Se1 Nb1 Se1 83.73(2) 14_566 14_666 ? Se1 Nb1 Se1 134.672(10) 1_565 14_666 ? Se1 Nb1 Se1 79.18(3) 14_556 . ? Se1 Nb1 Se1 83.73(2) 1_665 . ? Se1 Nb1 Se1 134.672(10) 14_566 . ? Se1 Nb1 Se1 83.73(2) 1_565 . ? Se1 Nb1 Se1 134.672(10) 14_666 . ? Nb1 Se1 Nb1 83.73(2) 1_445 1_545 ? Nb1 Se1 Nb1 83.73(2) 1_445 . ? Nb1 Se1 Nb1 83.73(2) 1_545 . ? Nb1 Se1 Na1 136.82(4) 1_445 13_666 ? Nb1 Se1 Na1 136.82(4) 1_545 13_666 ? Nb1 Se1 Na1 86.71(17) . 13_666 ? Nb1 Se1 Na1 136.82(4) 1_445 13_656 ? Nb1 Se1 Na1 86.71(17) 1_545 13_656 ? Nb1 Se1 Na1 136.82(4) . 13_656 ? Na1 Se1 Na1 72.2(3) 13_666 13_656 ? Nb1 Se1 Na1 86.71(17) 1_445 13_556 ? Nb1 Se1 Na1 136.82(4) 1_545 13_556 ? Nb1 Se1 Na1 136.82(4) . 13_556 ? Na1 Se1 Na1 72.2(3) 13_666 13_556 ? Na1 Se1 Na1 72.2(3) 13_656 13_556 ? Nb1 Se1 Na1 172.09(17) 1_445 . ? Nb1 Se1 Na1 102.09(12) 1_545 . ? Nb1 Se1 Na1 102.09(12) . . ? Na1 Se1 Na1 39.634(10) 13_666 . ? Na1 Se1 Na1 39.634(10) 13_656 . ? Na1 Se1 Na1 85.38(2) 13_556 . ? Nb1 Se1 Na1 102.09(12) 1_445 1_455 ? Nb1 Se1 Na1 172.09(17) 1_545 1_455 ? Nb1 Se1 Na1 102.09(12) . 1_455 ? Na1 Se1 Na1 39.634(10) 13_666 1_455 ? Na1 Se1 Na1 85.38(2) 13_656 1_455 ? Na1 Se1 Na1 39.634(10) 13_556 1_455 ? Na1 Se1 Na1 71.6(3) . 1_455 ? Nb1 Se1 Na1 102.09(12) 1_445 1_445 ? Nb1 Se1 Na1 102.09(12) 1_545 1_445 ? Nb1 Se1 Na1 172.09(17) . 1_445 ? Na1 Se1 Na1 85.38(2) 13_666 1_445 ? Na1 Se1 Na1 39.634(10) 13_656 1_445 ? Na1 Se1 Na1 39.634(10) 13_556 1_445 ? Na1 Se1 Na1 71.6(3) . 1_445 ? Na1 Se1 Na1 71.6(3) 1_455 1_445 ? Se1 Na1 Se1 72.2(3) 13_666 13_656 ? Se1 Na1 Se1 72.2(3) 13_666 13_556 ? Se1 Na1 Se1 72.2(3) 13_656 13_556 ? Se1 Na1 Se1 140.366(10) 13_666 . ? Se1 Na1 Se1 140.366(11) 13_656 . ? Se1 Na1 Se1 94.62(2) 13_556 . ? Se1 Na1 Se1 140.366(11) 13_666 1_655 ? Se1 Na1 Se1 94.62(2) 13_656 1_655 ? Se1 Na1 Se1 140.366(11) 13_556 1_655 ? Se1 Na1 Se1 71.6(3) . 1_655 ? Se1 Na1 Se1 94.62(2) 13_666 1_665 ? Se1 Na1 Se1 140.366(10) 13_656 1_665 ? Se1 Na1 Se1 140.366(10) 13_556 1_665 ? Se1 Na1 Se1 71.6(3) . 1_665 ? Se1 Na1 Se1 71.6(3) 1_655 1_665 ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 1.033 _refine_diff_density_min -1.106 _refine_diff_density_rms 0.235 #===END data_nbs2na _database_code_CSD 195104 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'sodium niobium disulfide' _chemical_melting_point ? _chemical_formula_moiety 'Na0.51 Nb S2' _chemical_formula_sum 'Na0.51 Nb S2' _chemical_formula_weight 168.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3)/mmc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z' '-x+y, -x, z' 'x-y, x, z+1/2' 'y, -x+y, z+1/2' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' '-y, -x, -z+1/2' 'x, x-y, -z+1/2' '-x+y, y, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, -x, -z-1/2' '-y, x-y, -z-1/2' '-x+y, y, z' 'x, x-y, z' '-y, -x, z' 'y, x, z-1/2' '-x, -x+y, z-1/2' 'x-y, -y, z-1/2' _cell_length_a 3.3533(4) _cell_length_b 3.3533(4) _cell_length_c 14.547(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 141.66(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 392 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 28.1 _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour 'metallic grey' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 3.956 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 157 _exptl_absorpt_coefficient_mu 5.440 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5020 _exptl_absorpt_correction_T_max 0.7568 _exptl_absorpt_process_details 'Bruker SADABS v2.03 (2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 458 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 2 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.61 _diffrn_reflns_theta_max 28.09 _reflns_number_total 90 _reflns_number_gt 86 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOMS 4.1 (Dowty, 1998)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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^)+(0.0583P)^2^+0.1428P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.044(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 90 _refine_ls_number_parameters 11 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0206 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 S1 S 0.0000 0.0000 0.35653(11) 0.0066(5) Uani 1 6 d S . . Nb1 Nb 0.3333 0.6667 0.2500 0.0055(5) Uani 1 12 d S . . Na1 Na 0.6667 0.3333 0.4998(11) 0.016(4) Uani 0.250(13) 6 d SP . . 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 S1 0.0052(6) 0.0052(6) 0.0092(8) 0.000 0.000 0.0026(3) Nb1 0.0045(5) 0.0045(5) 0.0076(6) 0.000 0.000 0.0022(3) Na1 0.023(4) 0.023(4) 0.004(5) 0.000 0.000 0.011(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 S1 Nb1 2.4799(10) 1_445 ? S1 Nb1 2.4799(10) 1_545 ? S1 Nb1 2.4799(10) . ? S1 Na1 2.845(12) . ? S1 Na1 2.845(12) 1_455 ? S1 Na1 2.845(12) 1_445 ? S1 Na1 2.849(12) 13_666 ? S1 Na1 2.849(12) 13_656 ? S1 Na1 2.849(12) 13_556 ? Nb1 S1 2.4799(10) 14_556 ? Nb1 S1 2.4799(10) 1_665 ? Nb1 S1 2.4799(10) 14_566 ? Nb1 S1 2.4799(10) 1_565 ? Nb1 S1 2.4799(10) 14_666 ? Nb1 Nb1 3.3533(4) 1_665 ? Nb1 Nb1 3.3533(4) 1_445 ? Nb1 Nb1 3.3533(4) 1_565 ? Nb1 Nb1 3.3533(4) 1_545 ? Nb1 Nb1 3.3533(4) 1_455 ? Nb1 Nb1 3.3533(4) 1_655 ? Na1 S1 2.845(12) 1_655 ? Na1 S1 2.845(12) 1_665 ? Na1 S1 2.849(12) 13_666 ? Na1 S1 2.849(12) 13_656 ? Na1 S1 2.849(12) 13_556 ? Na1 Nb1 3.639(16) 13_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 Nb1 S1 Nb1 85.08(4) 1_445 1_545 ? Nb1 S1 Nb1 85.08(4) 1_445 . ? Nb1 S1 Nb1 85.08(4) 1_545 . ? Nb1 S1 Na1 171.6(2) 1_445 . ? Nb1 S1 Na1 101.08(16) 1_545 . ? Nb1 S1 Na1 101.08(16) . . ? Nb1 S1 Na1 101.08(16) 1_445 1_455 ? Nb1 S1 Na1 171.6(2) 1_545 1_455 ? Nb1 S1 Na1 101.08(16) . 1_455 ? Na1 S1 Na1 72.2(4) . 1_455 ? Nb1 S1 Na1 101.08(16) 1_445 1_445 ? Nb1 S1 Na1 101.08(16) 1_545 1_445 ? Nb1 S1 Na1 171.6(2) . 1_445 ? Na1 S1 Na1 72.2(4) . 1_445 ? Na1 S1 Na1 72.2(4) 1_455 1_445 ? Nb1 S1 Na1 136.36(5) 1_445 13_666 ? Nb1 S1 Na1 136.36(5) 1_545 13_666 ? Nb1 S1 Na1 85.9(2) . 13_666 ? Na1 S1 Na1 39.759(18) . 13_666 ? Na1 S1 Na1 39.759(18) 1_455 13_666 ? Na1 S1 Na1 85.70(4) 1_445 13_666 ? Nb1 S1 Na1 136.36(5) 1_445 13_656 ? Nb1 S1 Na1 85.9(2) 1_545 13_656 ? Nb1 S1 Na1 136.36(5) . 13_656 ? Na1 S1 Na1 39.759(18) . 13_656 ? Na1 S1 Na1 85.70(4) 1_455 13_656 ? Na1 S1 Na1 39.759(18) 1_445 13_656 ? Na1 S1 Na1 72.1(4) 13_666 13_656 ? Nb1 S1 Na1 85.9(2) 1_445 13_556 ? Nb1 S1 Na1 136.36(5) 1_545 13_556 ? Nb1 S1 Na1 136.36(5) . 13_556 ? Na1 S1 Na1 85.70(4) . 13_556 ? Na1 S1 Na1 39.759(18) 1_455 13_556 ? Na1 S1 Na1 39.759(18) 1_445 13_556 ? Na1 S1 Na1 72.1(4) 13_666 13_556 ? Na1 S1 Na1 72.1(4) 13_656 13_556 ? S1 Nb1 S1 134.05(2) 14_556 1_665 ? S1 Nb1 S1 85.08(4) 14_556 14_566 ? S1 Nb1 S1 134.05(2) 1_665 14_566 ? S1 Nb1 S1 134.05(2) 14_556 1_565 ? S1 Nb1 S1 85.08(4) 1_665 1_565 ? S1 Nb1 S1 77.35(6) 14_566 1_565 ? S1 Nb1 S1 85.08(4) 14_556 14_666 ? S1 Nb1 S1 77.35(6) 1_665 14_666 ? S1 Nb1 S1 85.08(4) 14_566 14_666 ? S1 Nb1 S1 134.05(2) 1_565 14_666 ? S1 Nb1 S1 77.35(6) 14_556 . ? S1 Nb1 S1 85.08(4) 1_665 . ? S1 Nb1 S1 134.05(2) 14_566 . ? S1 Nb1 S1 85.08(4) 1_565 . ? S1 Nb1 S1 134.05(2) 14_666 . ? S1 Nb1 Nb1 132.54(2) 14_556 1_665 ? S1 Nb1 Nb1 47.46(2) 1_665 1_665 ? S1 Nb1 Nb1 90.0 14_566 1_665 ? S1 Nb1 Nb1 90.0 1_565 1_665 ? S1 Nb1 Nb1 47.46(2) 14_666 1_665 ? S1 Nb1 Nb1 132.54(2) . 1_665 ? S1 Nb1 Nb1 47.46(2) 14_556 1_445 ? S1 Nb1 Nb1 132.54(2) 1_665 1_445 ? S1 Nb1 Nb1 90.0 14_566 1_445 ? S1 Nb1 Nb1 90.0 1_565 1_445 ? S1 Nb1 Nb1 132.54(2) 14_666 1_445 ? S1 Nb1 Nb1 47.46(2) . 1_445 ? Nb1 Nb1 Nb1 180.0 1_665 1_445 ? S1 Nb1 Nb1 132.54(2) 14_556 1_565 ? S1 Nb1 Nb1 90.0 1_665 1_565 ? S1 Nb1 Nb1 47.46(2) 14_566 1_565 ? S1 Nb1 Nb1 47.46(2) 1_565 1_565 ? S1 Nb1 Nb1 90.0 14_666 1_565 ? S1 Nb1 Nb1 132.54(2) . 1_565 ? Nb1 Nb1 Nb1 60.0 1_665 1_565 ? Nb1 Nb1 Nb1 120.0 1_445 1_565 ? S1 Nb1 Nb1 47.46(2) 14_556 1_545 ? S1 Nb1 Nb1 90.0 1_665 1_545 ? S1 Nb1 Nb1 132.54(2) 14_566 1_545 ? S1 Nb1 Nb1 132.54(2) 1_565 1_545 ? S1 Nb1 Nb1 90.0 14_666 1_545 ? S1 Nb1 Nb1 47.46(2) . 1_545 ? Nb1 Nb1 Nb1 120.0 1_665 1_545 ? Nb1 Nb1 Nb1 60.0 1_445 1_545 ? Nb1 Nb1 Nb1 180.0 1_565 1_545 ? S1 Nb1 Nb1 90.0 14_556 1_455 ? S1 Nb1 Nb1 132.54(2) 1_665 1_455 ? S1 Nb1 Nb1 47.46(2) 14_566 1_455 ? S1 Nb1 Nb1 47.46(2) 1_565 1_455 ? S1 Nb1 Nb1 132.54(2) 14_666 1_455 ? S1 Nb1 Nb1 90.0 . 1_455 ? Nb1 Nb1 Nb1 120.0 1_665 1_455 ? Nb1 Nb1 Nb1 60.0 1_445 1_455 ? Nb1 Nb1 Nb1 60.0 1_565 1_455 ? Nb1 Nb1 Nb1 120.0 1_545 1_455 ? S1 Nb1 Nb1 90.0 14_556 1_655 ? S1 Nb1 Nb1 47.46(2) 1_665 1_655 ? S1 Nb1 Nb1 132.54(2) 14_566 1_655 ? S1 Nb1 Nb1 132.54(2) 1_565 1_655 ? S1 Nb1 Nb1 47.46(2) 14_666 1_655 ? S1 Nb1 Nb1 90.0 . 1_655 ? Nb1 Nb1 Nb1 60.0 1_665 1_655 ? Nb1 Nb1 Nb1 120.0 1_445 1_655 ? Nb1 Nb1 Nb1 120.0 1_565 1_655 ? Nb1 Nb1 Nb1 60.0 1_545 1_655 ? Nb1 Nb1 Nb1 180.0 1_455 1_655 ? S1 Na1 S1 72.2(4) . 1_655 ? S1 Na1 S1 72.2(4) . 1_665 ? S1 Na1 S1 72.2(4) 1_655 1_665 ? S1 Na1 S1 140.241(18) . 13_666 ? S1 Na1 S1 140.241(18) 1_655 13_666 ? S1 Na1 S1 94.30(5) 1_665 13_666 ? S1 Na1 S1 140.241(18) . 13_656 ? S1 Na1 S1 94.30(4) 1_655 13_656 ? S1 Na1 S1 140.241(18) 1_665 13_656 ? S1 Na1 S1 72.1(4) 13_666 13_656 ? S1 Na1 S1 94.30(5) . 13_556 ? S1 Na1 S1 140.241(18) 1_655 13_556 ? S1 Na1 S1 140.241(18) 1_665 13_556 ? S1 Na1 S1 72.1(4) 13_666 13_556 ? S1 Na1 S1 72.1(4) 13_656 13_556 ? S1 Na1 Nb1 137.1(2) . 13_666 ? S1 Na1 Nb1 137.1(2) 1_655 13_666 ? S1 Na1 Nb1 137.1(2) 1_665 13_666 ? S1 Na1 Nb1 42.8(2) 13_666 13_666 ? S1 Na1 Nb1 42.8(2) 13_656 13_666 ? S1 Na1 Nb1 42.8(2) 13_556 13_666 ? _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 0.641 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.159 #===END