#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:51:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179427 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/24/4332474.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332474
loop_
_publ_author_name
'Hanauer, Tobias'
'Aschenbrenner, Jürgen C.'
'Korber, Nikolaus'
_publ_section_title
;
 Dimers of Heptapnictide Anions:  As144-and P144-in the Crystal
 Structures of [Rb(18-crown-6)]4As14·6NH3and
 [Li(NH3)4]4P14·NH3
;
_journal_issue                   17
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6723
_journal_page_last               6727
_journal_paper_doi               10.1021/ic060418j
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'P14, 18(H3 N), 4(Li)'
_chemical_formula_sum            'H54 Li4 N18 P14'
_chemical_formula_weight         767.95
_chemical_name_systematic
; 
 Tetrakis(Tetraamminelithium)Tetradekaphosphide-Ammonia(1/1) 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.24(3)
_cell_angle_beta                 91.66(3)
_cell_angle_gamma                118.45(3)
_cell_formula_units_Z            1
_cell_length_a                   9.283(3)
_cell_length_b                   9.508(3)
_cell_length_c                   13.466(4)
_cell_measurement_reflns_used    5987
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      2.51
_cell_volume                     1023.8(6)
_computing_cell_refinement       'Stoe IPDS Software Vers2.89'
_computing_data_collection       'Stoe IPDS Software Vers2.89'
_computing_data_reduction        'Stoe IPDS Software Vers2.89'
_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 0.946
_diffrn_measured_fraction_theta_max 0.946
_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  0.0674
_diffrn_reflns_av_sigmaI/netI    0.0780
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5987
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DelRefAbs from Platon'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             402
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0409
_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/[σ²(Fo²)+(0.0588P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                2057
_reflns_number_total             2785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060418jsup2.cif
_cod_data_source_block           H54Li4N18P14
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4332474
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
P1 P 0.66422(14) 0.79613(13) 0.61820(7) 0.0254(3) Uani 1 1 d .
P2 P 0.62619(12) 0.55479(13) 0.54149(7) 0.0185(3) Uani 1 1 d .
P3 P 0.45181(14) 0.74013(15) 0.69787(8) 0.0305(3) Uani 1 1 d .
P4 P 0.85772(13) 0.83546(14) 0.73206(8) 0.0272(3) Uani 1 1 d .
P5 P 0.55018(13) 0.42069(13) 0.66537(7) 0.0208(3) Uani 1 1 d .
P6 P 0.45618(13) 0.55936(15) 0.77013(7) 0.0271(3) Uani 1 1 d .
P7 P 0.72239(13) 0.62075(14) 0.79343(7) 0.0249(3) Uani 1 1 d .
Li1 Li 0.3382(9) 0.1426(9) 0.9245(5) 0.0296(16) Uani 1 1 d .
N1 N 0.5688(4) 0.3406(4) 0.9665(2) 0.0293(8) Uani 1 1 d .
H1A H 0.6449 0.3063 0.9688 0.044 Uiso 1 1 calc R
H1B H 0.5723 0.3968 1.0288 0.044 Uiso 1 1 calc R
H1C H 0.5916 0.4068 0.9206 0.044 Uiso 1 1 calc R
N2 N 0.3125(4) 0.0292(4) 0.7759(2) 0.0287(8) Uani 1 1 d .
H2A H 0.3584 0.1059 0.7370 0.043 Uiso 1 1 calc R
H2B H 0.2034 -0.0367 0.7530 0.043 Uiso 1 1 calc R
H2C H 0.3643 -0.0318 0.7721 0.043 Uiso 1 1 calc R
N3 N 0.1624(5) 0.2185(5) 0.9152(3) 0.0371(9) Uani 1 1 d .
H3A H 0.1967 0.2991 0.8787 0.056 Uiso 1 1 calc R
H3B H 0.1493 0.2571 0.9787 0.056 Uiso 1 1 calc R
H3C H 0.0645 0.1326 0.8843 0.056 Uiso 1 1 calc R
N4 N 0.3022(5) 0.0096(5) 1.0385(3) 0.0374(9) Uani 1 1 d .
H4A H 0.2413 -0.0989 1.0114 0.056 Uiso 1 1 calc R
H4B H 0.2479 0.0383 1.0858 0.056 Uiso 1 1 calc R
H4C H 0.4018 0.0311 1.0682 0.056 Uiso 1 1 calc R
Li2 Li 0.9050(9) 0.2816(9) 0.6263(5) 0.0330(17) Uani 1 1 d .
N5 N 0.7861(5) 0.2246(5) 0.7541(3) 0.0335(9) Uani 1 1 d .
H5A H 0.7104 0.2597 0.7581 0.050 Uiso 1 1 calc R
H5B H 0.8615 0.2745 0.8105 0.050 Uiso 1 1 calc R
H5C H 0.7342 0.1146 0.7498 0.050 Uiso 1 1 calc R
N6 N 1.0072(5) 0.5272(5) 0.6279(3) 0.0338(9) Uani 1 1 d .
H6A H 0.9573 0.5425 0.5746 0.051 Uiso 1 1 calc R
H6B H 1.1171 0.5700 0.6229 0.051 Uiso 1 1 calc R
H6C H 0.9923 0.5777 0.6869 0.051 Uiso 1 1 calc R
N7 N 1.0757(5) 0.2013(5) 0.6165(3) 0.0427(10) Uani 1 1 d .
H7A H 1.0338 0.1031 0.6358 0.064 Uiso 1 1 calc R
H7B H 1.1697 0.2749 0.6579 0.064 Uiso 1 1 calc R
H7C H 1.0988 0.1903 0.5514 0.064 Uiso 1 1 calc R
N8 N 0.7272(7) 0.1477(6) 0.5048(3) 0.0775(18) Uani 1 1 d .
H8A H 0.6869 0.2103 0.4843 0.116 Uiso 1 1 calc R
H8B H 0.6437 0.0589 0.5230 0.116 Uiso 1 1 calc R
H8C H 0.7719 0.1145 0.4530 0.116 Uiso 1 1 calc R
N9 N 0.1017(10) 0.6315(9) 0.9097(7) 0.125(4) Uani 1 1 d G
H9A H 0.1344 0.5937 0.8741 0.188 Uiso 1 1 d G
H9B H 0.0234 0.6245 0.8799 0.188 Uiso 1 1 d G
H9C H 0.0490 0.5666 0.9375 0.188 Uiso 1 1 d G
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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'
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_3
P3 P1 P4 104.74(6) .
P3 P1 P2 104.30(7) .
P4 P1 P2 94.20(7) .
P5 P2 P1 100.27(6) .
P5 P2 P2 96.05(7) 2_666
P1 P2 P2 101.32(8) 2_666
P6 P3 P1 98.93(6) .
P7 P4 P1 98.43(7) .
P2 P5 P7 98.60(6) .
P2 P5 P6 104.18(6) .
P7 P5 P6 60.13(5) .
P3 P6 P5 107.84(6) .
P3 P6 P7 106.29(7) .
P5 P6 P7 59.83(6) .
P4 P7 P5 107.38(6) .
P4 P7 P6 105.72(6) .
P5 P7 P6 60.05(6) .
N1 Li1 N2 111.2(3) .
N1 Li1 N4 104.7(3) .
N2 Li1 N4 119.2(4) .
N1 Li1 N3 110.2(4) .
N2 Li1 N3 100.5(3) .
N4 Li1 N3 111.1(3) .
Li1 N1 H1A 109.5 .
Li1 N1 H1B 109.5 .
H1A N1 H1B 109.5 .
Li1 N1 H1C 109.5 .
H1A N1 H1C 109.5 .
H1B N1 H1C 109.5 .
Li1 N2 H2A 109.5 .
Li1 N2 H2B 109.5 .
H2A N2 H2B 109.5 .
Li1 N2 H2C 109.5 .
H2A N2 H2C 109.5 .
H2B N2 H2C 109.5 .
Li1 N3 H3A 109.5 .
Li1 N3 H3B 109.5 .
H3A N3 H3B 109.5 .
Li1 N3 H3C 109.5 .
H3A N3 H3C 109.5 .
H3B N3 H3C 109.5 .
Li1 N4 H4A 109.5 .
Li1 N4 H4B 109.5 .
H4A N4 H4B 109.5 .
Li1 N4 H4C 109.5 .
H4A N4 H4C 109.5 .
H4B N4 H4C 109.5 .
N8 Li2 N6 110.8(3) .
N8 Li2 N7 106.9(4) .
N6 Li2 N7 112.9(4) .
N8 Li2 N5 105.8(4) .
N6 Li2 N5 110.5(4) .
N7 Li2 N5 109.7(3) .
Li2 N5 H5A 109.5 .
Li2 N5 H5B 109.5 .
H5A N5 H5B 109.5 .
Li2 N5 H5C 109.5 .
H5A N5 H5C 109.5 .
H5B N5 H5C 109.5 .
Li2 N6 H6A 109.5 .
Li2 N6 H6B 109.5 .
H6A N6 H6B 109.5 .
Li2 N6 H6C 109.5 .
H6A N6 H6C 109.5 .
H6B N6 H6C 109.5 .
Li2 N7 H7A 109.5 .
Li2 N7 H7B 109.5 .
H7A N7 H7B 109.5 .
Li2 N7 H7C 109.5 .
H7A N7 H7C 109.5 .
H7B N7 H7C 109.5 .
Li2 N8 H8A 109.5 .
Li2 N8 H8B 109.5 .
H8A N8 H8B 109.5 .
Li2 N8 H8C 109.5 .
H8A N8 H8C 109.5 .
H8B N8 H8C 109.5 .
H9A N9 H9B 105.9 .
H9A N9 H9C 104.9 .
H9B N9 H9C 91.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 P3 2.1513(18) .
P1 P4 2.1757(16) .
P1 P2 2.2143(17) .
P2 P5 2.1909(15) .
P2 P2 2.230(2) 2_666
P3 P6 2.1222(17) .
P4 P7 2.1417(18) .
P5 P7 2.244(2) .
P5 P6 2.2495(16) .
P6 P7 2.2512(18) .
Li1 N1 2.048(8) .
Li1 N2 2.064(8) .
Li1 N4 2.078(7) .
Li1 N3 2.083(7) .
N1 H1A 0.9100 .
N1 H1B 0.9100 .
N1 H1C 0.9100 .
N2 H2A 0.9100 .
N2 H2B 0.9100 .
N2 H2C 0.9100 .
N3 H3A 0.9100 .
N3 H3B 0.9100 .
N3 H3C 0.9100 .
N4 H4A 0.9100 .
N4 H4B 0.9100 .
N4 H4C 0.9100 .
Li2 N8 2.049(8) .
Li2 N6 2.056(8) .
Li2 N7 2.060(8) .
Li2 N5 2.077(7) .
N5 H5A 0.9100 .
N5 H5B 0.9100 .
N5 H5C 0.9100 .
N6 H6A 0.9100 .
N6 H6B 0.9100 .
N6 H6C 0.9100 .
N7 H7A 0.9100 .
N7 H7B 0.9100 .
N7 H7C 0.9100 .
N8 H8A 0.9100 .
N8 H8B 0.9100 .
N8 H8C 0.9100 .
N9 H9A 0.7125 .
N9 H9B 0.7884 .
N9 H9C 0.7472 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A N9 0.91 2.59 3.316(6) 137.4 2_667
N4 H4A N9 0.91 2.39 3.291(7) 168.6 1_545
