#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:41:47 +0100 (lun 21 de mar de 2016) $
#$Revision: 178790 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/44/4104486.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_4104486
loop_
_publ_author_name
'Keith Huynh'
'Alan J. Lough'
'Michelle A. M. Forgeron'
'Martin Bendle'
'Alejandro Presa Soto'
'Roderick E. Wasylishen'
'Ian Manners'
_publ_section_title
;
 Synthesis and Reactivity of Phosphine-Stabilized Phosphoranimine Cations,
 [R3P.PR'2=NSiMe3]+
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7905
_journal_page_last               7916
_journal_paper_doi               10.1021/ja900256g
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C8 H24 N4 P4'
_chemical_formula_sum            'C8 H24 N4 P4'
_chemical_formula_weight         300.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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            4
_cell_length_a                   15.7111(8)
_cell_length_b                   15.7111(8)
_cell_length_c                   6.4101(4)
_cell_measurement_reflns_used    3062
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     1582.26(15)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3062
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  0.350
_exptl_absorpt_correction_T_min  0.250
_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    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0032(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0354
_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)+(0.0289P)²+2.2147P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                720
_reflns_number_total             898
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja900256g_si_008.cif
_cod_data_source_block           k0624
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4104486
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'
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 0.06514(3) 0.13794(3) 0.09144(8) 0.0241(2) Uani 1 1 d .
N1 N -0.03423(10) 0.14075(11) 0.0420(3) 0.0286(4) Uani 1 1 d .
C1 C 0.08957(15) 0.04690(13) 0.2492(4) 0.0388(6) Uani 1 1 d .
H1A H 0.0622 0.0529 0.3858 0.058 Uiso 1 1 calc R
H1B H 0.1514 0.0427 0.2677 0.058 Uiso 1 1 calc R
H1D H 0.0685 -0.0047 0.1804 0.058 Uiso 1 1 calc R
C2 C 0.11405(15) 0.11474(17) -0.1553(4) 0.0413(6) Uani 1 1 d .
H2B H 0.1032 0.1616 -0.2526 0.062 Uiso 1 1 calc R
H2C H 0.0901 0.0620 -0.2119 0.062 Uiso 1 1 calc R
H2D H 0.1756 0.1079 -0.1361 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
P1 0.0209(3) 0.0216(3) 0.0297(3) -0.0039(2) -0.0015(2) 0.00096(19)
N1 0.0213(9) 0.0289(9) 0.0355(10) -0.0093(8) 0.0004(7) -0.0010(7)
C1 0.0436(13) 0.0231(11) 0.0497(14) -0.0014(10) -0.0120(11) -0.0006(9)
C2 0.0282(12) 0.0532(15) 0.0426(14) -0.0134(11) 0.0064(10) -0.0013(11)
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'
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'
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
N1 P1 N1 119.90(12) 16
N1 P1 C1 104.75(10) 16
N1 P1 C1 110.12(10) .
N1 P1 C2 112.53(10) 16
N1 P1 C2 104.46(10) .
C1 P1 C2 104.08(12) .
P1 N1 P1 132.16(11) 15
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 N1 1.5917(17) 16
P1 N1 1.5937(17) .
P1 C1 1.794(2) .
P1 C2 1.796(2) .
N1 P1 1.5917(17) 15
