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_4301533
_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         '3(Rb +), (H2P3 3-), (H3N)'
_chemical_formula_sum            'H5 N P3 Rb3'
_chemical_formula_weight         368.37
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Trisrubidium catena-dihydrogentriphosphide ammonia(1/1) 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.971(2)
_cell_length_b                   9.6590(10)
_cell_length_c                   15.085(3)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.70
_cell_volume                     1890.0(5)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       Phi
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1435
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30514
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         2.70
_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    15.896
_exptl_absorpt_correction_T_max  0.1913
_exptl_absorpt_correction_T_min  0.0894
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   X-Red/X-Shape
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.589
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.550
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.228
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         2259
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                1547
_reflns_number_total             2259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8014546_si_002_3.cif
_cod_data_source_block           Rb3P3H2NH3
_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_database_code               4301533