#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:10:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179365 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/62/4326238.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_4326238
loop_
_publ_author_name
'Zin-Min Tun'
'Amy J. Heston'
'Matthew J. Panzner'
'Doug A. Medvetz'
'Brian D. Wright'
'Deepa Savant'
'Venkat R. Dudipala'
'Debasish Banerjee'
'Peter L. Rinaldi'
'Wiley J. Youngs'
'Claire A. Tessier'
_publ_section_title
;
 Group 13 Lewis Acid Adducts of [PCl2N]3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8937
_journal_page_last               8945
_journal_paper_doi               10.1021/ic201075z
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'Al Br3 Cl6 N3 P3'
_chemical_formula_sum            'Al Br3 Cl6 N3 P3'
_chemical_formula_weight         614.35
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.898(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8919(12)
_cell_length_b                   12.1067(14)
_cell_length_c                   12.1387(14)
_cell_measurement_reflns_used    5713
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.38
_cell_volume                     1599.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12824
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         26.30
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    8.898
_exptl_absorpt_correction_T_max  0.766
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.551
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0202
_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)+(0.0225P)²+0.7312P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0450
_refine_ls_wR_factor_ref         0.0465
_reflns_number_gt                3059
_reflns_number_total             3402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201075z_si_002_1.cif
_cod_data_source_block           '[PCl2N]3.AlBr3'
_cod_database_code               4326238
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
Br1 Br 0.00549(2) 0.90051(2) 0.38320(2) 0.02053(7) Uani 1 1 d .
Br2 Br 0.18306(3) 0.7500 0.16339(3) 0.01815(8) Uani 1 2 d S
Br3 Br 0.41380(2) 0.40171(2) -0.19360(2) 0.02065(7) Uani 1 1 d .
Br4 Br 0.56146(3) 0.2500 0.05105(3) 0.02123(9) Uani 1 2 d S
P1 P 0.34175(5) 0.86640(5) 0.46966(5) 0.01257(13) Uani 1 1 d .
P2 P 0.55306(8) 0.7500 0.52687(7) 0.01320(18) Uani 1 2 d S
P3 P 0.19115(6) 0.13313(5) 0.03615(5) 0.01431(13) Uani 1 1 d .
P4 P 0.04339(8) 0.2500 0.17784(7) 0.01691(19) Uani 1 2 d S
Al1 Al 0.11859(9) 0.7500 0.33895(8) 0.0132(2) Uani 1 2 d S
Al2 Al 0.41144(9) 0.2500 -0.08336(8) 0.0141(2) Uani 1 2 d S
N1 N 0.48279(18) 0.86026(17) 0.49667(17) 0.0167(4) Uani 1 1 d .
N2 N 0.2741(2) 0.7500 0.4305(2) 0.0131(6) Uani 1 2 d S
N3 N 0.1025(2) 0.14003(18) 0.13456(18) 0.0227(5) Uani 1 1 d .
N4 N 0.2572(2) 0.2500 0.0004(2) 0.0124(6) Uani 1 2 d S
Cl1 Cl 0.25477(6) 0.92401(5) 0.59816(5) 0.02191(14) Uani 1 1 d .
Cl2 Cl 0.31097(5) 0.97517(5) 0.35265(5) 0.01850(13) Uani 1 1 d .
Cl3 Cl 0.59447(8) 0.7500 0.68850(7) 0.01999(18) Uani 1 2 d S
Cl4 Cl 0.71378(7) 0.7500 0.45837(7) 0.02045(19) Uani 1 2 d S
Cl5 Cl 0.10486(6) 0.07128(5) -0.09537(5) 0.02310(14) Uani 1 1 d .
Cl6 Cl 0.32248(6) 0.02740(5) 0.07380(5) 0.02142(14) Uani 1 1 d .
Cl7 Cl 0.05110(9) 0.2500 0.34027(7) 0.0295(2) Uani 1 2 d S
Cl8 Cl -0.13584(8) 0.2500 0.14382(8) 0.0314(2) Uani 1 2 d S
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'
Al Al 0.0645 0.0514 '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'
Br Br -0.2901 2.4595 '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
N1 P1 N2 116.48(12) . .
N1 P1 Cl2 109.14(8) . .
N2 P1 Cl2 107.53(9) . .
N1 P1 Cl1 110.16(8) . .
N2 P1 Cl1 107.84(10) . .
Cl2 P1 Cl1 105.07(4) . .
N1 P2 N1 115.79(15) 4_575 .
N1 P2 Cl4 109.55(8) 4_575 .
N1 P2 Cl4 109.55(8) . .
N1 P2 Cl3 108.69(8) 4_575 .
N1 P2 Cl3 108.69(8) . .
Cl4 P2 Cl3 103.91(5) . .
N3 P3 N4 116.14(12) . .
N3 P3 Cl6 108.71(9) . .
N4 P3 Cl6 107.42(9) . .
N3 P3 Cl5 110.43(9) . .
N4 P3 Cl5 108.20(10) . .
Cl6 P3 Cl5 105.36(4) . .
N3 P4 N3 115.21(16) . 4_565
N3 P4 Cl7 109.21(9) . .
N3 P4 Cl7 109.21(9) 4_565 .
N3 P4 Cl8 109.94(9) . .
N3 P4 Cl8 109.94(9) 4_565 .
Cl7 P4 Cl8 102.56(5) . .
N2 Al1 Br2 103.91(9) . .
N2 Al1 Br1 108.96(5) . 4_575
Br2 Al1 Br1 114.16(3) . 4_575
N2 Al1 Br1 108.96(5) . .
Br2 Al1 Br1 114.16(3) . .
Br1 Al1 Br1 106.52(4) 4_575 .
N4 Al2 Br4 103.43(9) . .
N4 Al2 Br3 109.06(5) . 4_565
Br4 Al2 Br3 113.65(3) . 4_565
N4 Al2 Br3 109.06(5) . .
Br4 Al2 Br3 113.65(3) . .
Br3 Al2 Br3 107.80(4) 4_565 .
P1 N1 P2 123.77(13) . .
P1 N2 P1 117.01(17) 4_575 .
P1 N2 Al1 121.49(8) 4_575 .
P1 N2 Al1 121.49(8) . .
P3 N3 P4 124.71(14) . .
P3 N4 P3 117.85(16) 4_565 .
P3 N4 Al2 121.08(8) 4_565 .
P3 N4 Al2 121.08(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Al1 2.2738(7) .
Br2 Al1 2.2658(11) .
Br3 Al2 2.2731(7) .
Br4 Al2 2.2705(11) .
P1 N1 1.562(2) .
P1 N2 1.6527(15) .
P1 Cl2 1.9576(8) .
P1 Cl1 1.9786(9) .
P2 N1 1.576(2) 4_575
P2 N1 1.576(2) .
P2 Cl4 1.9627(12) .
P2 Cl3 1.9986(12) .
P3 N3 1.563(2) .
P3 N4 1.6520(15) .
P3 Cl6 1.9622(9) .
P3 Cl5 1.9732(9) .
P4 N3 1.577(2) .
P4 N3 1.577(2) 4_565
P4 Cl7 1.9707(13) .
P4 Cl8 1.9820(13) .
Al1 N2 1.995(3) .
Al1 Br1 2.2738(7) 4_575
Al2 N4 1.992(3) .
Al2 Br3 2.2731(7) 4_565
N2 P1 1.6527(15) 4_575
N4 P3 1.6520(15) 4_565
