#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:54:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179134 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/96/4309613.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_4309613
loop_
_publ_author_name
'Amy J. Heston'
'Matthew J. Panzner'
'Wiley J. Youngs'
'Claire A. Tessier'
_publ_section_title
;
Lewis Acid Adducts of [PCl2N]3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6518
_journal_page_last               6520
_journal_paper_doi               10.1021/ic050974y
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'Cl9 Ga N3 P3'
_chemical_formula_weight         523.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 91.989(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.7624(11)
_cell_length_b                   10.7999(10)
_cell_length_c                   23.873(2)
_cell_measurement_temperature    100(2)
_cell_volume                     3030.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            26454
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    3.693
_exptl_absorpt_correction_T_max  0.8663
_exptl_absorpt_correction_T_min  0.4245
_exptl_crystal_density_diffrn    2.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         7291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0405
_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/[σ²(Fo²)+(0.0338P)²+2.2738P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                6270
_reflns_number_total             7291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050974ysi20050615_080523.cif
_cod_data_source_block           mp
_cod_database_code               4309613
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 1.09580(3) 0.07383(3) 0.130985(17) 0.01460(10) Uani 1 1 d . . .
Ga2 Ga 0.34042(3) 0.61163(3) 0.118369(16) 0.01229(9) Uani 1 1 d . . .
Cl1 Cl 0.93602(8) 0.18821(8) 0.24145(4) 0.02191(19) Uani 1 1 d . . .
Cl2 Cl 1.11818(9) 0.38841(8) 0.21596(4) 0.0256(2) Uani 1 1 d . . .
Cl3 Cl 0.93444(8) 0.16828(8) 0.01420(4) 0.02086(19) Uani 1 1 d . . .
Cl4 Cl 1.11198(8) 0.37904(9) 0.03713(4) 0.0243(2) Uani 1 1 d . . .
Cl5 Cl 0.66351(8) 0.45551(9) 0.12044(5) 0.0294(2) Uani 1 1 d . . .
Cl6 Cl 0.86227(8) 0.64291(8) 0.11937(5) 0.0264(2) Uani 1 1 d . . .
Cl7 Cl 1.20094(8) 0.07749(9) 0.20607(4) 0.0243(2) Uani 1 1 d . . .
Cl8 Cl 0.96240(8) -0.06163(8) 0.13083(5) 0.0260(2) Uani 1 1 d . . .
Cl9 Cl 1.20015(8) 0.06671(8) 0.05885(4) 0.0223(2) Uani 1 1 d . . .
Cl10 Cl 0.34858(8) 0.80169(8) 0.23571(4) 0.01916(19) Uani 1 1 d . . .
Cl11 Cl 0.60235(8) 0.73915(8) 0.21511(4) 0.02098(19) Uani 1 1 d . . .
Cl12 Cl 0.35333(7) 0.81493(8) 0.00801(3) 0.01640(18) Uani 1 1 d . . .
Cl13 Cl 0.60683(7) 0.75236(8) 0.03660(4) 0.01942(18) Uani 1 1 d . . .
Cl14 Cl 0.45670(8) 1.21318(8) 0.12890(4) 0.01966(19) Uani 1 1 d . . .
Cl15 Cl 0.69497(8) 1.08897(9) 0.13451(4) 0.0234(2) Uani 1 1 d . . .
Cl16 Cl 0.38978(8) 0.50336(8) 0.19073(4) 0.02131(19) Uani 1 1 d . . .
Cl17 Cl 0.16749(7) 0.67462(8) 0.11776(4) 0.01984(19) Uani 1 1 d . . .
Cl18 Cl 0.38682(8) 0.51182(8) 0.04480(4) 0.02016(19) Uani 1 1 d . . .
P1 P 0.97712(8) 0.31161(8) 0.18511(4) 0.01514(19) Uani 1 1 d . . .
P2 P 0.97433(8) 0.30208(8) 0.06689(4) 0.01383(18) Uani 1 1 d . . .
P3 P 0.83121(8) 0.46288(8) 0.12178(4) 0.01624(19) Uani 1 1 d . . .
P4 P 0.47061(8) 0.83340(8) 0.18353(4) 0.01297(18) Uani 1 1 d . . .
P5 P 0.47400(7) 0.84179(8) 0.06542(4) 0.01150(18) Uani 1 1 d . . .
P6 P 0.52923(8) 1.04918(8) 0.12885(4) 0.01348(18) Uani 1 1 d . . .
N1 N 1.0084(2) 0.2379(3) 0.12741(12) 0.0136(6) Uani 1 1 d . . .
N2 N 0.8751(3) 0.3986(3) 0.06732(13) 0.0209(7) Uani 1 1 d . . .
N3 N 0.8793(3) 0.4084(3) 0.17918(13) 0.0270(8) Uani 1 1 d . . .
N4 N 0.4340(2) 0.7715(2) 0.12275(12) 0.0128(6) Uani 1 1 d . . .
N5 N 0.5017(2) 0.9831(3) 0.07107(12) 0.0147(6) Uani 1 1 d . . .
N6 N 0.4970(3) 0.9752(3) 0.18285(12) 0.0176(6) 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
N N 0.0061 0.0033 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ga1 Cl7 107.04(8) . . ?
N1 Ga1 Cl8 102.95(9) . . ?
Cl7 Ga1 Cl8 114.52(4) . . ?
N1 Ga1 Cl9 107.27(8) . . ?
Cl7 Ga1 Cl9 109.98(4) . . ?
Cl8 Ga1 Cl9 114.33(4) . . ?
N4 Ga2 Cl17 103.93(8) . . ?
N4 Ga2 Cl18 108.28(8) . . ?
Cl17 Ga2 Cl18 114.94(4) . . ?
N4 Ga2 Cl16 106.73(8) . . ?
Cl17 Ga2 Cl16 114.06(4) . . ?
Cl18 Ga2 Cl16 108.36(4) . . ?
N3 P1 N1 115.81(16) . . ?
N3 P1 Cl1 108.60(14) . . ?
N1 P1 Cl1 108.23(11) . . ?
N3 P1 Cl2 111.11(15) . . ?
N1 P1 Cl2 107.82(12) . . ?
Cl1 P1 Cl2 104.65(6) . . ?
N2 P2 N1 115.81(16) . . ?
N2 P2 Cl3 109.44(13) . . ?
N1 P2 Cl3 107.42(11) . . ?
N2 P2 Cl4 110.07(13) . . ?
N1 P2 Cl4 108.44(11) . . ?
Cl3 P2 Cl4 105.09(6) . . ?
N2 P3 N3 115.75(16) . . ?
N2 P3 Cl5 108.93(13) . . ?
N3 P3 Cl5 109.10(14) . . ?
N2 P3 Cl6 110.03(13) . . ?
N3 P3 Cl6 109.28(14) . . ?
Cl5 P3 Cl6 102.98(6) . . ?
N6 P4 N4 115.86(15) . . ?
N6 P4 Cl10 109.10(12) . . ?
N4 P4 Cl10 108.33(11) . . ?
N6 P4 Cl11 110.77(13) . . ?
N4 P4 Cl11 107.76(11) . . ?
Cl10 P4 Cl11 104.38(6) . . ?
N5 P5 N4 116.24(15) . . ?
N5 P5 Cl12 110.36(12) . . ?
N4 P5 Cl12 106.95(11) . . ?
N5 P5 Cl13 109.94(12) . . ?
N4 P5 Cl13 108.39(11) . . ?
Cl12 P5 Cl13 104.23(5) . . ?
N6 P6 N5 116.03(15) . . ?
N6 P6 Cl14 109.87(12) . . ?
N5 P6 Cl14 109.40(12) . . ?
N6 P6 Cl15 108.45(13) . . ?
N5 P6 Cl15 109.09(12) . . ?
Cl14 P6 Cl15 103.22(5) . . ?
P2 N1 P1 118.60(17) . . ?
P2 N1 Ga1 120.62(16) . . ?
P1 N1 Ga1 120.70(16) . . ?
P2 N2 P3 124.3(2) . . ?
P1 N3 P3 124.8(2) . . ?
P4 N4 P5 118.20(17) . . ?
P4 N4 Ga2 120.84(16) . . ?
P5 N4 Ga2 120.96(15) . . ?
P5 N5 P6 123.52(18) . . ?
P4 N6 P6 124.01(19) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ga1 N1 2.049(3) . ?
Ga1 Cl7 2.1425(10) . ?
Ga1 Cl8 2.1451(10) . ?
Ga1 Cl9 2.1505(10) . ?
Ga2 N4 2.048(3) . ?
Ga2 Cl17 2.1444(9) . ?
Ga2 Cl18 2.1473(9) . ?
Ga2 Cl16 2.1492(9) . ?
Cl1 P1 1.9658(13) . ?
Cl2 P1 1.9744(13) . ?
Cl3 P2 1.9618(12) . ?
Cl4 P2 1.9741(13) . ?
Cl5 P3 1.9733(13) . ?
Cl6 P3 1.9795(13) . ?
Cl10 P4 1.9631(13) . ?
Cl11 P4 1.9811(12) . ?
Cl12 P5 1.9601(12) . ?
Cl13 P5 1.9803(12) . ?
Cl14 P6 1.9660(12) . ?
Cl15 P6 1.9963(13) . ?
P1 N3 1.558(3) . ?
P1 N1 1.644(3) . ?
P2 N2 1.565(3) . ?
P2 N1 1.640(3) . ?
P3 N2 1.576(3) . ?
P3 N3 1.578(3) . ?
P4 N6 1.563(3) . ?
P4 N4 1.641(3) . ?
P5 N5 1.566(3) . ?
P5 N4 1.648(3) . ?
P6 N6 1.574(3) . ?
P6 N5 1.577(3) . ?
