#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/11/10/4111032.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_4111032
loop_
_publ_author_name
'Keith Huynh'
'Alan J. Lough'
'Ian Manners'
_publ_section_title
;
 Reactions of P-Donor Ligands with
 N-Silyl(halogeno)organophosphoranimines: Formation of Cations with P-P
 Coordination Bonds and Poly(alkyl/aryl)phosphazenes at Ambient
 Temperature
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14002
_journal_page_last               14003
_journal_paper_doi               10.1021/ja063979i
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C8 H24 N P2 Si, Br'
_chemical_formula_sum            'C8 H24 Br N P2 Si'
_chemical_formula_weight         304.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_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                   11.7432(2)
_cell_length_b                   11.5531(4)
_cell_length_c                   22.8714(9)
_cell_measurement_reflns_used    23642
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     3102.97(17)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2003)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'SHELXTL V6.1'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1(Sheldrick, 2001)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_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  0.0686
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23642
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.902
_exptl_absorpt_correction_T_max  0.657
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         3544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0704
_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/[σ²(Fo²)+(0.0471P)²+0.7610P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                2449
_reflns_number_total             3544
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja063979isi20060606_013231.cif
_cod_data_source_block           k0615a
_cod_database_code               4111032
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, 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
Br1 Br 0.21184(2) 0.43963(2) 0.753731(14) 0.04546(14) Uani 1 1 d .
P1 P -0.05574(6) 0.24335(6) 0.61859(3) 0.0383(2) Uani 1 1 d .
P2 P 0.06220(6) 0.14151(6) 0.67456(3) 0.0367(2) Uani 1 1 d .
Si1 Si 0.05516(7) 0.24472(6) 0.49700(4) 0.0392(2) Uani 1 1 d .
N1 N -0.0315(2) 0.2147(2) 0.55434(11) 0.0467(6) Uani 1 1 d .
C1 C 0.1499(3) 0.3720(3) 0.51094(15) 0.0556(8) Uani 1 1 d .
H1A H 0.1035 0.4421 0.5148 0.083 Uiso 1 1 calc R
H1B H 0.2030 0.3812 0.4782 0.083 Uiso 1 1 calc R
H1C H 0.1929 0.3594 0.5471 0.083 Uiso 1 1 calc R
C2 C 0.1448(3) 0.1151(2) 0.48031(14) 0.0486(8) Uani 1 1 d .
H2A H 0.0966 0.0459 0.4794 0.073 Uiso 1 1 calc R
H2B H 0.2031 0.1062 0.5106 0.073 Uiso 1 1 calc R
H2C H 0.1816 0.1253 0.4422 0.073 Uiso 1 1 calc R
C3 C -0.0346(3) 0.2787(3) 0.43195(15) 0.0547(9) Uani 1 1 d .
H3A H -0.0753 0.3516 0.4386 0.082 Uiso 1 1 calc R
H3B H -0.0898 0.2162 0.4258 0.082 Uiso 1 1 calc R
H3C H 0.0140 0.2861 0.3973 0.082 Uiso 1 1 calc R
C4 C -0.1927(2) 0.1972(3) 0.64401(14) 0.0474(8) Uani 1 1 d .
H4A H -0.2523 0.2351 0.6209 0.071 Uiso 1 1 calc R
H4B H -0.2015 0.2182 0.6853 0.071 Uiso 1 1 calc R
H4C H -0.1993 0.1130 0.6397 0.071 Uiso 1 1 calc R
C5 C -0.0371(2) 0.3893(2) 0.64349(15) 0.0461(8) Uani 1 1 d .
H5A H -0.0828 0.4416 0.6193 0.069 Uiso 1 1 calc R
H5B H 0.0435 0.4107 0.6405 0.069 Uiso 1 1 calc R
H5C H -0.0616 0.3953 0.6843 0.069 Uiso 1 1 calc R
C6 C 0.2039(2) 0.1849(2) 0.65572(14) 0.0429(7) Uani 1 1 d .
H6A H 0.2588 0.1329 0.6745 0.064 Uiso 1 1 calc R
H6B H 0.2171 0.2643 0.6691 0.064 Uiso 1 1 calc R
H6C H 0.2135 0.1812 0.6132 0.064 Uiso 1 1 calc R
C7 C 0.0426(2) -0.0058(2) 0.65246(15) 0.0466(8) Uani 1 1 d .
H7A H 0.1018 -0.0541 0.6702 0.070 Uiso 1 1 calc R
H7B H 0.0477 -0.0111 0.6098 0.070 Uiso 1 1 calc R
H7C H -0.0325 -0.0327 0.6653 0.070 Uiso 1 1 calc R
C8 C 0.0392(2) 0.1573(3) 0.75134(12) 0.0412(7) Uani 1 1 d .
H8A H 0.0939 0.1091 0.7727 0.062 Uiso 1 1 calc R
H8B H -0.0384 0.1329 0.7610 0.062 Uiso 1 1 calc R
H8C H 0.0496 0.2385 0.7624 0.062 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.03636(19) 0.0401(2) 0.0599(2) -0.00336(13) -0.00302(15) -0.00077(11)
P1 0.0327(4) 0.0392(4) 0.0432(5) -0.0002(3) 0.0002(3) -0.0016(3)
P2 0.0317(4) 0.0359(4) 0.0425(4) -0.0034(3) -0.0001(3) -0.0019(3)
Si1 0.0385(5) 0.0358(4) 0.0433(5) -0.0023(3) 0.0014(4) -0.0010(3)
N1 0.0454(15) 0.0498(14) 0.0450(16) -0.0024(12) 0.0002(12) -0.0100(11)
C1 0.055(2) 0.0455(17) 0.066(2) -0.0024(15) 0.0107(17) -0.0068(15)
C2 0.0443(19) 0.0414(16) 0.060(2) -0.0019(14) 0.0017(15) 0.0038(13)
C3 0.063(2) 0.0537(19) 0.048(2) -0.0016(15) -0.0040(16) 0.0116(15)
C4 0.0336(17) 0.0552(18) 0.053(2) 0.0083(15) 0.0011(14) -0.0028(13)
C5 0.0446(18) 0.0399(16) 0.054(2) -0.0011(14) 0.0005(15) -0.0001(12)
C6 0.0301(15) 0.0481(16) 0.0504(18) -0.0004(14) 0.0010(13) -0.0019(12)
C7 0.0421(18) 0.0396(16) 0.058(2) -0.0084(14) -0.0022(15) 0.0015(12)
C8 0.0404(17) 0.0407(16) 0.0426(18) -0.0040(12) 0.0025(13) -0.0058(12)
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'
Br Br -0.2901 2.4595 '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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N1 P1 C4 114.43(14)
N1 P1 C5 118.99(15)
C4 P1 C5 106.65(15)
N1 P1 P2 108.81(11)
C4 P1 P2 102.41(11)
C5 P1 P2 103.79(11)
C8 P2 C7 110.80(15)
C8 P2 C6 110.39(14)
C7 P2 C6 108.53(14)
C8 P2 P1 114.72(11)
C7 P2 P1 105.08(11)
C6 P2 P1 107.00(10)
N1 Si1 C3 108.69(16)
N1 Si1 C2 109.40(14)
C3 Si1 C2 108.90(15)
N1 Si1 C1 112.68(14)
C3 Si1 C1 107.86(16)
C2 Si1 C1 109.22(15)
P1 N1 Si1 143.98(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
P1 N1 1.533(3)
P1 C4 1.792(3)
P1 C5 1.793(3)
P1 P2 2.2229(11)
P2 C8 1.786(3)
P2 C7 1.790(3)
P2 C6 1.791(3)
Si1 N1 1.696(3)
Si1 C3 1.865(3)
Si1 C2 1.870(3)
Si1 C1 1.872(3)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660175
