#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:26:20 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179449 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/46/4334680.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4334680
loop_
_publ_author_name
'Christian Hering'
'Axel Schulz'
'Alexander Villinger'
_publ_contact_author_address
;
Universität Rostock
Institut für Chemie
Abteilung für Anorganische Chemie
Albert-Einstein-Strasse 3a 
18059 Rostock
Bundesrepublik Deutschland
;
_publ_contact_author_email
;
axel.schulz@uni-rostock.de'
;
_publ_contact_author_fax         '+49 (0)381/498-6382'
_publ_contact_author_name        'Axel Schulz'
_publ_contact_author_phone       '+49 (0)381/498-6400'
_publ_section_title
;
 On the Synthesis and Reactivity of Highly Labile Pseudohalogen
 Phosphenium Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5214
_journal_page_last               5225
_journal_paper_doi               10.1021/ic4001285
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C13 H28 N6 P Si2 +, Cl4 Ga -'
_chemical_formula_sum            'C13 H28 Cl4 Ga N6 P Si2'
_chemical_formula_weight         567.08
_chemical_name_systematic
;
N,N-bis(trimethylsilyl)amino(4-dimethylaminopyridyl)azidophosphenium 
tetrachlorogallate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.644(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9817(3)
_cell_length_b                   26.1792(8)
_cell_length_c                   10.0690(3)
_cell_measurement_reflns_used    3873
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      43.635
_cell_measurement_theta_min      4.386
_cell_volume                     2618.40(14)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            23933
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    1.623
_exptl_absorpt_correction_T_max  0.9379
_exptl_absorpt_correction_T_min  0.5850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         4101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0347
_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)+(0.0271P)²+1.2506P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                2847
_reflns_number_total             4101
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic4001285_si_002_07.cif
_cod_data_source_block           ch100_npn3_dmap_gacl4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4334680
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.83262(11) 0.12230(4) 0.53808(9) 0.0398(3) Uani 1 1 d .
N1 N 0.9131(4) 0.15235(13) 0.4116(3) 0.0526(10) Uani 1 1 d .
N2 N 0.8436(4) 0.16981(14) 0.3246(3) 0.0559(10) Uani 1 1 d .
N3 N 0.7842(5) 0.18978(17) 0.2340(4) 0.0989(16) Uani 1 1 d .
N4 N 0.8383(3) 0.16484(10) 0.6593(2) 0.0318(7) Uani 1 1 d .
N5 N 0.9803(3) 0.08370(11) 0.5842(3) 0.0337(7) Uani 1 1 d .
N6 N 1.2895(3) -0.01743(11) 0.7007(3) 0.0385(8) Uani 1 1 d .
Si1 Si 0.97348(12) 0.21053(4) 0.69029(10) 0.0430(3) Uani 1 1 d .
Si2 Si 0.68677(11) 0.17020(4) 0.74101(9) 0.0358(3) Uani 1 1 d .
C1 C 0.9346(5) 0.26613(14) 0.5802(4) 0.0591(13) Uani 1 1 d .
H1A H 0.9360 0.2557 0.4869 0.089 Uiso 1 1 calc R
H1B H 1.0020 0.2929 0.6014 0.089 Uiso 1 1 calc R
H1C H 0.8451 0.2793 0.5940 0.089 Uiso 1 1 calc R
C2 C 0.9859(5) 0.22980(16) 0.8683(4) 0.0613(13) Uani 1 1 d .
H2A H 0.9003 0.2448 0.8886 0.092 Uiso 1 1 calc R
H2B H 1.0581 0.2550 0.8856 0.092 Uiso 1 1 calc R
H2C H 1.0059 0.1997 0.9248 0.092 Uiso 1 1 calc R
C3 C 1.1385(4) 0.18320(16) 0.6588(5) 0.0634(13) Uani 1 1 d .
H3A H 1.1586 0.1537 0.7173 0.095 Uiso 1 1 calc R
H3B H 1.2088 0.2091 0.6769 0.095 Uiso 1 1 calc R
H3C H 1.1356 0.1723 0.5654 0.095 Uiso 1 1 calc R
C4 C 0.6316(4) 0.23771(14) 0.7410(4) 0.0540(12) Uani 1 1 d .
H4A H 0.7007 0.2584 0.7918 0.081 Uiso 1 1 calc R
H4B H 0.5470 0.2402 0.7823 0.081 Uiso 1 1 calc R
H4C H 0.6180 0.2502 0.6490 0.081 Uiso 1 1 calc R
C5 C 0.7173(4) 0.14465(15) 0.9121(3) 0.0430(10) Uani 1 1 d .
H5A H 0.7523 0.1097 0.9089 0.064 Uiso 1 1 calc R
H5B H 0.6327 0.1444 0.9539 0.064 Uiso 1 1 calc R
H5C H 0.7831 0.1662 0.9644 0.064 Uiso 1 1 calc R
C6 C 0.5501(4) 0.13199(17) 0.6513(4) 0.0574(12) Uani 1 1 d .
H6A H 0.5380 0.1425 0.5575 0.086 Uiso 1 1 calc R
H6B H 0.4662 0.1376 0.6922 0.086 Uiso 1 1 calc R
H6C H 0.5738 0.0957 0.6569 0.086 Uiso 1 1 calc R
C7 C 1.0713(4) 0.06910(15) 0.4996(3) 0.0418(10) Uani 1 1 d .
H7 H 1.0628 0.0825 0.4115 0.050 Uiso 1 1 calc R
C8 C 1.1722(4) 0.03675(14) 0.5351(3) 0.0387(10) Uani 1 1 d .
H8 H 1.2341 0.0284 0.4726 0.046 Uiso 1 1 calc R
C9 C 1.1885(4) 0.01469(14) 0.6640(3) 0.0342(9) Uani 1 1 d .
C10 C 1.0911(4) 0.02876(14) 0.7491(3) 0.0369(9) Uani 1 1 d .
H10 H 1.0944 0.0146 0.8362 0.044 Uiso 1 1 calc R
C11 C 0.9924(4) 0.06241(14) 0.7078(3) 0.0364(9) Uani 1 1 d .
H11 H 0.9289 0.0715 0.7680 0.044 Uiso 1 1 calc R
C12 C 1.3993(4) -0.02423(15) 0.6163(4) 0.0480(11) Uani 1 1 d .
H12A H 1.3625 -0.0356 0.5273 0.072 Uiso 1 1 calc R
H12B H 1.4623 -0.0500 0.6561 0.072 Uiso 1 1 calc R
H12C H 1.4466 0.0083 0.6088 0.072 Uiso 1 1 calc R
C13 C 1.3076(4) -0.04063(16) 0.8336(4) 0.0541(12) Uani 1 1 d .
H13A H 1.3515 -0.0161 0.8973 0.081 Uiso 1 1 calc R
H13B H 1.3638 -0.0712 0.8309 0.081 Uiso 1 1 calc R
H13C H 1.2196 -0.0501 0.8615 0.081 Uiso 1 1 calc R
Ga1 Ga 0.25103(4) 0.082150(16) 0.13304(4) 0.03785(14) Uani 1 1 d .
Cl1 Cl 0.33210(12) 0.12691(4) 0.30302(9) 0.0537(3) Uani 1 1 d .
Cl2 Cl 0.03734(11) 0.09665(5) 0.09390(11) 0.0675(4) Uani 1 1 d .
Cl3 Cl 0.35295(12) 0.09796(4) -0.04160(10) 0.0577(3) Uani 1 1 d .
Cl4 Cl 0.27945(11) 0.00170(4) 0.18510(10) 0.0501(3) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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
N4 P1 N1 104.44(16)
N4 P1 N5 102.67(14)
N1 P1 N5 90.97(15)
N2 N1 P1 116.3(3)
N1 N2 N3 173.6(5)
P1 N4 Si2 115.01(16)
P1 N4 Si1 123.03(17)
Si2 N4 Si1 121.14(15)
C11 N5 C7 117.0(3)
C11 N5 P1 117.5(2)
C7 N5 P1 125.0(2)
C9 N6 C12 120.2(3)
C9 N6 C13 122.4(3)
C12 N6 C13 116.6(3)
N4 Si1 C1 107.97(17)
N4 Si1 C3 112.12(17)
C1 Si1 C3 109.8(2)
N4 Si1 C2 108.94(16)
C1 Si1 C2 110.84(19)
C3 Si1 C2 107.1(2)
N4 Si2 C5 109.27(16)
N4 Si2 C4 109.78(16)
C5 Si2 C4 111.57(17)
N4 Si2 C6 110.31(16)
C5 Si2 C6 107.79(19)
C4 Si2 C6 108.1(2)
Si1 C1 H1A 109.5
Si1 C1 H1B 109.5
H1A C1 H1B 109.5
Si1 C1 H1C 109.5
H1A C1 H1C 109.5
H1B C1 H1C 109.5
Si1 C2 H2A 109.5
Si1 C2 H2B 109.5
H2A C2 H2B 109.5
Si1 C2 H2C 109.5
H2A C2 H2C 109.5
H2B C2 H2C 109.5
Si1 C3 H3A 109.5
Si1 C3 H3B 109.5
H3A C3 H3B 109.5
Si1 C3 H3C 109.5
H3A C3 H3C 109.5
H3B C3 H3C 109.5
Si2 C4 H4A 109.5
Si2 C4 H4B 109.5
H4A C4 H4B 109.5
Si2 C4 H4C 109.5
H4A C4 H4C 109.5
H4B C4 H4C 109.5
Si2 C5 H5A 109.5
Si2 C5 H5B 109.5
H5A C5 H5B 109.5
Si2 C5 H5C 109.5
H5A C5 H5C 109.5
H5B C5 H5C 109.5
Si2 C6 H6A 109.5
Si2 C6 H6B 109.5
H6A C6 H6B 109.5
Si2 C6 H6C 109.5
H6A C6 H6C 109.5
H6B C6 H6C 109.5
C8 C7 N5 122.9(3)
C8 C7 H7 118.6
N5 C7 H7 118.6
C7 C8 C9 121.3(3)
C7 C8 H8 119.4
C9 C8 H8 119.4
N6 C9 C10 122.9(3)
N6 C9 C8 121.8(3)
C10 C9 C8 115.3(4)
C11 C10 C9 120.5(3)
C11 C10 H10 119.8
C9 C10 H10 119.8
C10 C11 N5 123.0(3)
C10 C11 H11 118.5
N5 C11 H11 118.5
N6 C12 H12A 109.5
N6 C12 H12B 109.5
H12A C12 H12B 109.5
N6 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
N6 C13 H13A 109.5
N6 C13 H13B 109.5
H13A C13 H13B 109.5
N6 C13 H13C 109.5
H13A C13 H13C 109.5
H13B C13 H13C 109.5
Cl3 Ga1 Cl2 110.70(5)
Cl3 Ga1 Cl1 111.79(4)
Cl2 Ga1 Cl1 109.52(5)
Cl3 Ga1 Cl4 108.69(4)
Cl2 Ga1 Cl4 108.39(5)
Cl1 Ga1 Cl4 107.63(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
P1 N4 1.649(3)
P1 N1 1.757(3)
P1 N5 1.810(3)
N1 N2 1.157(4)
N2 N3 1.162(5)
N4 Si2 1.797(3)
N4 Si1 1.808(3)
N5 C11 1.358(4)
N5 C7 1.359(4)
N6 C9 1.337(4)
N6 C12 1.463(4)
N6 C13 1.464(4)
Si1 C1 1.847(4)
Si1 C3 1.852(4)
Si1 C2 1.855(4)
Si2 C5 1.845(3)
Si2 C4 1.851(4)
Si2 C6 1.853(4)
C1 H1A 0.9800
C1 H1B 0.9800
C1 H1C 0.9800
C2 H2A 0.9800
C2 H2B 0.9800
C2 H2C 0.9800
C3 H3A 0.9800
C3 H3B 0.9800
C3 H3C 0.9800
C4 H4A 0.9800
C4 H4B 0.9800
C4 H4C 0.9800
C5 H5A 0.9800
C5 H5B 0.9800
C5 H5C 0.9800
C6 H6A 0.9800
C6 H6B 0.9800
C6 H6C 0.9800
C7 C8 1.337(5)
C7 H7 0.9500
C8 C9 1.415(5)
C8 H8 0.9500
C9 C10 1.408(5)
C10 C11 1.356(5)
C10 H10 0.9500
C11 H11 0.9500
C12 H12A 0.9800
C12 H12B 0.9800
C12 H12C 0.9800
C13 H13A 0.9800
C13 H13B 0.9800
C13 H13C 0.9800
Ga1 Cl3 2.1564(11)
Ga1 Cl2 2.1642(12)
Ga1 Cl1 2.1644(10)
Ga1 Cl4 2.1822(11)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N4 P1 N1 N2 -100.5(3)
N5 P1 N1 N2 156.2(3)
P1 N1 N2 N3 165(4)
N1 P1 N4 Si2 138.47(18)
N5 P1 N4 Si2 -127.18(16)
N1 P1 N4 Si1 -31.2(2)
N5 P1 N4 Si1 63.1(2)
N4 P1 N5 C11 55.1(3)
N1 P1 N5 C11 160.1(3)
N4 P1 N5 C7 -133.6(3)
N1 P1 N5 C7 -28.6(3)
P1 N4 Si1 C1 85.0(2)
Si2 N4 Si1 C1 -84.1(2)
P1 N4 Si1 C3 -36.2(3)
Si2 N4 Si1 C3 154.7(2)
P1 N4 Si1 C2 -154.6(2)
Si2 N4 Si1 C2 36.3(2)
P1 N4 Si2 C5 110.34(19)
Si1 N4 Si2 C5 -79.7(2)
P1 N4 Si2 C4 -127.00(19)
Si1 N4 Si2 C4 42.9(2)
P1 N4 Si2 C6 -8.0(2)
Si1 N4 Si2 C6 161.94(19)
C11 N5 C7 C8 -2.4(5)
P1 N5 C7 C8 -173.7(3)
N5 C7 C8 C9 1.4(6)
C12 N6 C9 C10 -170.2(3)
C13 N6 C9 C10 -0.3(6)
C12 N6 C9 C8 10.2(5)
C13 N6 C9 C8 -179.9(3)
C7 C8 C9 N6 -179.6(4)
C7 C8 C9 C10 0.8(5)
N6 C9 C10 C11 178.5(3)
C8 C9 C10 C11 -1.8(5)
C9 C10 C11 N5 0.9(6)
C7 N5 C11 C10 1.3(5)
P1 N5 C11 C10 173.3(3)
