Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_[Na(NH~3~)~5~][Na(NH~3~)~3~(P~3~H~3~)] _database_code_CSD 158623 _journal_coden_Cambridge 186 _publ_requested_journal ; Journal of the Chemical Society, Dalton Transactions ; _publ_contact_author ; Prof. Dr. Nikolaus Korber Institut f. Anorganische Chemie, Universit\"at Regensburg 93040 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 loop_ _publ_author_name _publ_author_address 'Korber, Nikolaus' ; Institut f. Anorg. Chemie der Universit\"at Regensburg 93040 Regensburg Germany ; 'Aschenbrenner, Jurgen' ; Institut f. Anorg. Chemie der Universit\"at Regensburg 93040 Regensburg Germany ; _publ_section_title ; The first catena-Trihydrogen Triphosphide: Synthesis and Crystal Structure of [Na(NH~3~)~5~][Na(NH~3~)~3~(P~3~H~3~)] ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dinatrium trihydrogentriphosphide-ammonia(1/8) ; _chemical_formula_moiety '(H15 N5 Na +), (H12 N3 Na P3 -)' _chemical_formula_sum 'H27 N8 Na2 P3' _chemical_formula_weight 278.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'P' 'P' 0.1023 0.0942 '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 'P21/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.3400(7) _cell_length_b 10.2514(8) _cell_length_c 10.8730(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.500(10) _cell_angle_gamma 90.00 _cell_volume 812.88(12) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7316 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 25.8 _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 0.997 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 260 _exptl_absorpt_coefficient_mu 0.392 _exptl_absorpt_correction_type none _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 11470 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.96 _reflns_number_total 1660 _reflns_number_gt 1298 _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 SHELXL97' _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^)+(0.0483P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_number_reflns 1660 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.108 _refine_ls_shift/su_mean 0.012 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 P1 P 0.16269(7) 0.07111(5) 0.79415(4) 0.02000(15) Uani 1 1 d . . . H1 H 0.049(4) 0.028(3) 0.877(3) 0.053(8) Uiso 1 1 d . . . P2 P 0.00932(9) 0.2500 0.73945(6) 0.01980(18) Uani 1 2 d S . . H2 H 0.033(5) 0.2500 0.617(3) 0.037(10) Uiso 1 2 d S . . Na1 Na -0.66275(14) 0.2500 0.44489(9) 0.0202(2) Uani 1 2 d S . . Na2 Na 0.37631(15) 0.2500 0.98747(10) 0.0267(3) Uani 1 2 d S . . N1 N -0.7456(3) 0.01579(19) 0.46595(18) 0.0265(4) Uani 1 1 d . . . H1A H -0.786(4) 0.012(3) 0.530(3) 0.036(7) Uiso 1 1 d . . . H1B H -0.847(4) -0.009(3) 0.405(3) 0.050(8) Uiso 1 1 d . . . H1C H -0.667(4) -0.049(4) 0.472(3) 0.055(9) Uiso 1 1 d . . . N2 N 0.3633(3) 0.0632(2) 1.1365(2) 0.0295(4) Uani 1 1 d . . . H2A H 0.465(4) 0.015(3) 1.140(2) 0.039(7) Uiso 1 1 d . . . H2B H 0.348(6) 0.067(5) 1.213(4) 0.104(16) Uiso 1 1 d . . . H2C H 0.287(6) 0.022(4) 1.107(4) 0.086(14) Uiso 1 1 d . . . N3 N -0.4927(3) 0.2500 0.6579(2) 0.0222(5) Uani 1 2 d S . . H3A H -0.371(6) 0.2500 0.682(3) 0.035(10) Uiso 1 2 d S . . H3B H -0.538(4) 0.180(3) 0.694(3) 0.059(9) Uiso 1 1 d . . . N4 N -0.3803(4) 0.2500 0.3371(3) 0.0347(6) Uani 1 2 d S . . H4A H -0.292(11) 0.2500 0.391(7) 0.13(3) Uiso 1 2 d S . . H4B H -0.350(5) 0.180(4) 0.306(4) 0.078(12) Uiso 1 1 d . . . N5 N -0.9167(3) 0.2500 0.2724(2) 0.0241(5) Uani 1 2 d S . . H5A H -0.988(4) 0.185(3) 0.270(3) 0.048(8) Uiso 1 1 d . . . H5B H -0.886(6) 0.2500 0.194(4) 0.053(12) Uiso 1 2 d S . . N6 N 0.7167(4) 0.2500 1.0042(3) 0.0293(6) Uani 1 2 d S . . H6A H 0.768(4) 0.181(3) 1.046(3) 0.061(9) Uiso 1 1 d . . . H6B H 0.761(7) 0.2500 0.940(5) 0.061(14) Uiso 1 2 d S . . 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 P1 0.0207(2) 0.0167(2) 0.0225(3) 0.00066(19) 0.00254(17) -0.00096(19) P2 0.0147(3) 0.0214(4) 0.0227(3) 0.000 -0.0004(2) 0.000 Na1 0.0198(5) 0.0206(6) 0.0198(5) 0.000 0.0002(4) 0.000 Na2 0.0246(6) 0.0335(7) 0.0215(5) 0.000 0.0007(4) 0.000 N1 0.0315(10) 0.0239(9) 0.0238(9) 0.0004(7) 0.0023(8) -0.0012(8) N2 0.0292(10) 0.0257(10) 0.0329(10) -0.0007(8) 0.0001(8) 0.0021(9) N3 0.0177(12) 0.0296(14) 0.0194(11) 0.000 0.0028(9) 0.000 N4 0.0371(16) 0.0325(17) 0.0377(16) 0.000 0.0187(13) 0.000 N5 0.0209(12) 0.0212(13) 0.0291(14) 0.000 -0.0021(10) 0.000 N6 0.0284(13) 0.0370(16) 0.0221(13) 0.000 0.0012(11) 0.000 _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 P1 P2 2.1982(6) . ? P1 Na2 3.0812(10) . ? P1 H1 1.37(3) . ? P2 P1 2.1982(6) 4_565 ? P2 H2 1.37(4) . ? Na1 N5 2.490(3) . ? Na1 N4 2.494(3) . ? Na1 N1 2.4936(19) . ? Na1 N1 2.4936(19) 4_565 ? Na1 N3 2.503(2) . ? Na2 N6 2.484(3) . ? Na2 N2 2.518(2) 4_565 ? Na2 N2 2.518(2) . ? Na2 P1 3.0812(10) 4_565 ? N1 H1A 0.79(3) . ? N1 H1B 0.97(3) . ? N1 H1C 0.88(4) . ? N2 H2A 0.90(3) . ? N2 H2B 0.85(5) . ? N2 H2C 0.74(5) . ? N3 H3A 0.90(4) . ? N3 H3B 0.90(3) . ? N4 H4A 0.82(8) . ? N4 H4B 0.83(4) . ? N5 H5A 0.85(3) . ? N5 H5B 0.90(5) . ? N6 H6A 0.91(4) . ? N6 H6B 0.81(5) . ? 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 P2 P1 Na2 83.89(3) . . ? P2 P1 H1 96.6(13) . . ? Na2 P1 H1 92.7(12) . . ? P1 P2 P1 113.07(4) 4_565 . ? P1 P2 H2 98.4(8) 4_565 . ? P1 P2 H2 98.4(8) . . ? N5 Na1 N4 103.73(11) . . ? N5 Na1 N1 84.24(5) . . ? N4 Na1 N1 105.51(5) . . ? N5 Na1 N1 84.24(5) . 4_565 ? N4 Na1 N1 105.51(5) . 4_565 ? N1 Na1 N1 148.67(10) . 4_565 ? N5 Na1 N3 161.65(10) . . ? N4 Na1 N3 94.62(10) . . ? N1 Na1 N3 90.93(5) . . ? N1 Na1 N3 90.93(5) 4_565 . ? N6 Na2 N2 93.67(7) . 4_565 ? N6 Na2 N2 93.67(7) . . ? N2 Na2 N2 99.04(11) 4_565 . ? N6 Na2 P1 118.68(6) . . ? N2 Na2 P1 146.97(6) 4_565 . ? N2 Na2 P1 86.16(5) . . ? N6 Na2 P1 118.68(6) . 4_565 ? N2 Na2 P1 86.16(5) 4_565 4_565 ? N2 Na2 P1 146.97(6) . 4_565 ? P1 Na2 P1 73.05(3) . 4_565 ? Na1 N1 H1A 104(2) . . ? Na1 N1 H1B 111.1(18) . . ? H1A N1 H1B 105(3) . . ? Na1 N1 H1C 125(2) . . ? H1A N1 H1C 102(3) . . ? H1B N1 H1C 108(3) . . ? Na2 N2 H2C 111.0(18) . . ? Na2 N2 H2B 127(3) . . ? H2C N2 H2B 101(3) . . ? Na2 N2 H2C 103(3) . . ? H2A N2 H2C 107(4) . . ? H2B N2 H2C 106(4) . . ? Na1 N3 H3A 130(2) . . ? Na1 N3 H3B 104(2) . . ? H3A N3 H3B 106(2) . . ? Na1 N4 H4A 107(5) . . ? Na1 N4 H4B 118(3) . . ? H4A N4 H4B 94(3) . . ? Na1 N5 H5A 115.4(19) . . ? Na1 N5 H5B 118(3) . . ? H5A N5 H5B 101(2) . . ? Na2 N6 H6A 113(2) . . ? Na2 N6 H6B 116(3) . . ? H6A N6 H6B 105(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.304 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.058