Hydrogen Polyphosphides P3H23- and P3H32-: Synthesis and Crystal Structure of K3(P3H2).2.3NH3, Rb3(P3H2).NH3, [Rb(18-crown-6)]2(P3H3).7.5NH3, and [Cs(18-crown-6)]2(P3H3).7NH3
Florian Kraus; Jürgen C. Aschenbrenner; T. Klamroth; Nikolaus Korber; Inorganic Chemistry 48 (2009) 1911–1919; doi:10.1021/ic8014546

data_4301532
_publ_contact_author_address
;
Institut f\"ur Anorganische Chemie
Universit\"at Regensburg
Universit\"atsstrasse 31
93053 Regensburg
GERMANY
;
_publ_contact_author_email       nikolaus.korber@chemie.uni-regensburg.de
_publ_contact_author_fax         '+49 941 9431812'
_publ_contact_author_name        'Nikolaus Korber'
_publ_contact_author_phone       '+49 941 9434448'
_publ_section_title
;
Hydrogen Polyphosphides P3H23- and P3H32-: Synthesis and Crystal
Structure of K3(P3H2).2.3NH3, Rb3(P3H2).NH3,
[Rb(18-crown-6)]2(P3H3).7.5NH3, and [Cs(18-crown-6)]2(P3H3).7NH3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1911
_journal_page_last               1919
_journal_paper_doi               10.1021/ic8014546
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '(K +)3, (H3P3 2-), 2.3(H3N)'
_chemical_formula_sum            'H9 K3 N2.33 P3'
_chemical_formula_weight         251.97
_chemical_melting_point          ?
_chemical_name_common
'Potassium dihydrogentriphosphide 2.3 ammoniate'
_chemical_name_systematic
'Trispotassium catena-trans-dihydrogentriphosphide ammonia(1/2.3)'
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   9.775(10)
_cell_length_b                   9.775(10)
_cell_length_c                   57.35(11)
_cell_measurement_temperature    123(2)
_cell_volume                     4746(11)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1998)'
_computing_data_reduction        IPDS
_computing_molecular_graphics    'Diamond V 2.1e'
_computing_publication_material  'CIFTAB in SHELXL 97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       Phi
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            8216
_diffrn_reflns_theta_full        23.97
_diffrn_reflns_theta_max         23.97
_diffrn_reflns_theta_min         2.51
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Stoe IPDS I'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.681
_exptl_absorpt_correction_T_max  0.726
_exptl_absorpt_correction_T_min  0.277
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DELrefABS in PLATON'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             2292
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.382
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.271
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         829
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1629P)^2^+22.0801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1981
_refine_ls_wR_factor_ref         0.2107
_reflns_number_gt                696
_reflns_number_total             829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8014546_si_002_2.cif
_cod_data_source_block           K3(P3H2)_2.3NH3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4746(12)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4301532