The first catena-trihydrogen triphosphide: synthesis and crystal structure of [Na(NH3)5][Na(NH3)3(P3H3)]
Korber, Nikolaus; Aschenbrenner, Jürgen; Journal of the Chemical Society, Dalton Transactions  (2001) 1165–; doi:10.1039/b101533h

data_7010637
_publ_contact_author
;
Prof. Dr. Nikolaus Korber
Institut f. Anorganische Chemie, Universit\"at Regensburg
93040 Regensburg
Germany
;
_publ_section_title
;
 The first catena-trihydrogen triphosphide: synthesis and crystal
 structure of [Na(NH3)5][Na(NH3)3(P3H3)]
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1165
_journal_paper_doi               10.1039/b101533h
_journal_year                    2001
_chemical_formula_moiety         '(H15 N5 Na +), (H12 N3 Na P3 -)'
_chemical_formula_sum            'H27 N8 Na2 P3'
_chemical_formula_weight         278.17
_chemical_name_systematic
; 
Dinatrium trihydrogentriphosphide-ammonia(1/8) 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.500(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.3400(7)
_cell_length_b                   10.2514(8)
_cell_length_c                   10.8730(10)
_cell_measurement_reflns_used    7316
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.8
_cell_measurement_theta_min      2.8
_cell_volume                     812.88(13)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1998)'
_computing_data_reduction        IPDS
_computing_publication_material  'CIFTAB in SHELXL97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       Phi
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11470
_diffrn_reflns_theta_full        25.96
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.997
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             260
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.108
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0787
_reflns_number_gt                1298
_reflns_number_total             1660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b101533h.txt
_cod_data_source_block           '[Na(NH~3~)~5~][Na(NH~3~)~3~(P~3~H~3~)]'
_cod_original_cell_volume        812.88(12)
_cod_original_sg_symbol_H-M      P21/m
_cod_database_code               7010637