Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_[Na(NH~3~)~5~]~2~[As~4~](NH~3~)~3~ _database_code_CSD 174984 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name _publ_author_address 'Korber, Nikolaus' ; Institut f. Anorg. Chemie der Universitat Regensburg 93040 Regensburg Germany ; 'Reil, Markus' ; Institut f. Anorg. Chemie der Universitat Regensburg 93040 Regensburg Germany ; _publ_contact_author_name 'Prof Nikolaus Korber' _publ_contact_author_address ; Institut für Anorganische Chemie Universität Regensburg Universitätsstraße 31 93053 Regensburg GERMANY ; _publ_contact_author_phone '+49 941 9434448' _publ_contact_author_fax '+49 941 9431812' _publ_contact_author_email nikolaus.korber@chemie.uni-regensburg.de _publ_section_title ; An Isolated Cyclo-Tetraarsendiide: Low Temperature Synthesis and Crystal Structure of Bis-Pentaamminesodium tetraarsendiide-ammonia(1/3) [Na(NH3)5]2As4 · 3 NH3 ; _audit_creation_method SHELXL-97 _chemical_name_systematic 'Bis (pentammin sodium) tetraarsenide-ammonia (1/3)' _chemical_formula_moiety '2(H15 N5 Na +), (As4 2-), 3 (H3 N)' _chemical_formula_sum 'H39 As4 N13 Na2' _chemical_formula_weight 567.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 12.042(1) _cell_length_b 12.287(1) _cell_length_c 16.122(1) _cell_angle_alpha 90.00 _cell_angle_beta 98.59(1) _cell_angle_gamma 90.00 _cell_volume 2358.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 2211 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 25.90 _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 5.662 _exptl_absorpt_correction_type empirical _exptl_special_details ; crystal mounting in perfluorether (T. Kottke, D. Stalke, J. Appl. Crystallogr. 26, 1993, p. 615) ; _diffrn_ambient_temperature 123(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 'Stoe Imaging Plate Diffraction System' _diffrn_measurement_method Phi _diffrn_reflns_number 16220 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.90 _reflns_number_total 2211 _reflns_number_gt 1230 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe & Cie, 1998)' _computing_cell_refinement 'IPDS' _computing_data_reduction 'IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'CIFTAB in SHELXL 97' _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^)+(0.0349P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2211 _refine_ls_number_parameters 106 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.885 _refine_ls_shift/su_max 0.001 _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 As1 As 0.2500 0.11928(5) 0.0000 0.0378(2) Uani 1 2 d S . . As2 As 0.14851(3) 0.25362(6) 0.05970(3) 0.04424(15) Uani 1 1 d . . . As3 As 0.2500 0.38811(6) 0.0000 0.0498(3) Uani 1 2 d S . . Na1 Na -0.03258(14) 0.03915(15) 0.22551(12) 0.0384(4) Uani 1 1 d . . . N1 N -0.1364(4) 0.1446(3) 0.0978(3) 0.0453(10) Uani 1 1 d . . . H1A H -0.1723 0.0966 0.0599 0.054 Uiso 1 1 calc R . . H1B H -0.0858 0.1836 0.0733 0.054 Uiso 1 1 calc R . . H1C H -0.1874 0.1906 0.1152 0.054 Uiso 1 1 calc R . . N2 N -0.2108(3) -0.0437(3) 0.2464(3) 0.0377(9) Uani 1 1 d . . . H2A H -0.2026 -0.0770 0.2974 0.045 Uiso 1 1 calc R . . H2B H -0.2316 -0.0937 0.2054 0.045 Uiso 1 1 calc R . . H2C H -0.2645 0.0088 0.2443 0.045 Uiso 1 1 calc R . . N3 N 0.0535(3) -0.0578(3) 0.1153(3) 0.0417(10) Uani 1 1 d . . . H3A H 0.1009 -0.1103 0.1395 0.050 Uiso 1 1 calc R . . H3B H 0.0925 -0.0095 0.0880 0.050 Uiso 1 1 calc R . . H3C H -0.0016 -0.0890 0.0780 0.050 Uiso 1 1 calc R . . N4 N 0.0652(3) -0.0687(3) 0.3459(3) 0.0420(10) Uani 1 1 d . . . H4A H 0.1034 -0.0229 0.3843 0.050 Uiso 1 1 calc R . . H4B H 0.1142 -0.1158 0.3271 0.050 Uiso 1 1 calc R . . H4C H 0.0137 -0.1068 0.3700 0.050 Uiso 1 1 calc R . . N5 N 0.0550(3) 0.2091(3) 0.2833(3) 0.0379(10) Uani 1 1 d . . . H5A H 0.0012 0.2610 0.2839 0.045 Uiso 1 1 calc R . . H5B H 0.1061 0.2320 0.2508 0.045 Uiso 1 1 calc R . . H5C H 0.0901 0.1973 0.3365 0.045 Uiso 1 1 calc R . . N6 N 0.1338(4) 0.6503(5) 0.0755(3) 0.0668(15) Uani 1 1 d D . . H6A H 0.043(3) 0.644(5) 0.056(4) 0.080 Uiso 1 1 d D . . H6B H 0.144(5) 0.564(3) 0.063(4) 0.080 Uiso 1 1 d D . . H6C H 0.177(5) 0.703(4) 0.124(3) 0.080 Uiso 1 1 d D . . N7 N 0.2218(6) 0.7699(8) 0.2394(7) 0.058(3) 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 As1 0.0458(5) 0.0245(4) 0.0425(6) 0.000 0.0044(4) 0.000 As2 0.0332(2) 0.0630(3) 0.0390(3) -0.0090(4) 0.01350(19) 0.0050(3) As3 0.0681(6) 0.0250(4) 0.0496(6) 0.000 -0.0131(5) 0.000 Na1 0.0388(10) 0.0419(9) 0.0346(11) 0.0018(8) 0.0050(8) -0.0067(8) N1 0.052(3) 0.048(2) 0.035(3) -0.0023(19) 0.007(2) -0.014(2) N2 0.0357(19) 0.0397(19) 0.037(2) 0.0056(18) 0.004(2) 0.0004(16) N3 0.036(2) 0.051(2) 0.037(2) 0.0004(19) 0.0035(18) -0.0083(19) N4 0.041(2) 0.039(2) 0.044(3) 0.0016(18) 0.001(2) -0.0063(18) N5 0.035(2) 0.0355(18) 0.041(2) 0.0032(16) 0.0011(19) 0.0017(15) N6 0.061(3) 0.085(4) 0.049(3) -0.014(3) -0.010(3) 0.011(3) N7 0.038(6) 0.066(8) 0.074(8) 0.014(5) 0.017(6) 0.011(4) _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 As1 As2 2.3444(8) 2 ? As1 As2 2.3444(8) . ? As2 As3 2.3457(8) . ? As3 As2 2.3457(8) 2 ? Na1 N2 2.443(4) . ? Na1 N5 2.459(4) . ? Na1 N3 2.490(5) . ? Na1 N4 2.495(4) . ? Na1 N1 2.591(4) . ? N7 N7 0.864(15) 7_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag As2 As1 As2 90.49(4) 2 . ? As1 As2 As3 89.54(2) . . ? As2 As3 As2 90.43(4) . 2 ? N2 Na1 N5 129.59(16) . . ? N2 Na1 N3 111.52(15) . . ? N5 Na1 N3 118.41(15) . . ? N2 Na1 N4 89.64(14) . . ? N5 Na1 N4 91.77(14) . . ? N3 Na1 N4 95.88(15) . . ? N2 Na1 N1 89.35(14) . . ? N5 Na1 N1 90.29(14) . . ? N3 Na1 N1 82.79(15) . . ? N4 Na1 N1 177.91(15) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.90 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.585 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.085