#------------------------------------------------------------------------------
#$Date: 2016-03-22 10:05:44 +0100 (mar 22 de mar de 2016) $
#$Revision: 178884 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/13/4111353.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_4111353
loop_
_publ_author_name
'Jan J. Weigand'
'Susanne D. Riegel'
'Neil Burford'
'Andreas Decken'
_publ_contact_author_address
;Department of Chemistry
University of New Brunswick
Fredericton, NB
E3B 6E2
Canada
;
_publ_contact_author_email       adecken@unb.ca
_publ_contact_author_fax         '(506) 453-4981'
_publ_contact_author_name        'Andreas Decken'
_publ_contact_author_phone       '(506) 453-4875'
_publ_section_title
;
 Prototypical Phosphorus Analogues of Ethane: General and Versatile
 Synthetic Approaches to Hexaalkylated P-P Diphosphonium Cations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7969
_journal_page_last               7976
_journal_paper_doi               10.1021/ja071306+
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C6 H18 P2, 2(C F3 O3 S) '
_chemical_formula_sum            'C8 H18 F6 O6 P2 S2'
_chemical_formula_weight         450.28
_space_group_IT_number           166
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      166
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   difmap
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   9.228(3)
_cell_length_b                   9.228(3)
_cell_length_c                   17.826(5)
_cell_measurement_reflns_used    1759
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.932
_cell_measurement_theta_min      2.792
_cell_volume                     1314.6(7)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            3007
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.79
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              K760
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.9721
_exptl_absorpt_correction_T_min  0.8258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997b)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       Plate
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.381
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.381
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0391
_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)+(0.0535P)²+1.1404P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                366
_reflns_number_total             399
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja071306si20070411_031725.cif
_cod_data_source_block           nb060750
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               4111353
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'-x, -x+y, -z'
'x-y, -y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'x, x-y, z'
'-x+y, y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
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
P P 0.3333 0.6667 0.10501(5) 0.0219(3) Uani 1 6 d S
C1 C 0.5466(3) 0.77331(17) 0.07567(14) 0.0322(6) Uani 1 2 d S
S S 1.0000 1.0000 0.21025(5) 0.0298(4) Uani 1 6 d S
F F 1.1557(2) 1.07783(10) 0.08117(8) 0.0372(5) Uani 1 2 d S
O O 0.8247(3) 0.91237(13) 0.22899(11) 0.0446(6) Uani 1 2 d S
C2 C 1.0000 1.0000 0.1081(2) 0.0270(9) Uani 1 6 d S
H1A H 0.552(5) 0.776(3) 0.018(2) 0.066(12) Uiso 1 2 d S
H1B H 0.605(3) 0.888(3) 0.0946(13) 0.049(6) Uiso 1 1 d .
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
P 0.0219(4) 0.0219(4) 0.0219(6) 0.000 0.000 0.0110(2)
C1 0.0243(12) 0.0385(11) 0.0291(12) 0.0012(5) 0.0024(9) 0.0121(6)
S 0.0328(5) 0.0328(5) 0.0239(6) 0.000 0.000 0.0164(2)
F 0.0309(9) 0.0395(7) 0.0384(8) 0.0051(3) 0.0102(6) 0.0155(4)
O 0.0365(11) 0.0533(11) 0.0383(11) 0.0059(4) 0.0119(8) 0.0183(6)
C2 0.0264(14) 0.0264(14) 0.028(2) 0.000 0.000 0.0132(7)
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 '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
C1 P C1 111.77(8) 2_665 .
C1 P P 107.06(9) . 25_565
P C1 H1A 110(2) . .
P C1 H1B 110.7(13) . .
H1A C1 H1B 109.0(18) . .
O S O 114.79(6) . 2_765
O S C2 103.42(9) . .
F C2 F 107.79(18) . 2_765
F C2 S 111.10(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P C1 1.783(3) .
P P 2.198(2) 25_565
C1 H1A 1.03(3) .
C1 H1B 0.97(2) .
S O 1.440(2) .
S C2 1.821(4) .
F C2 1.333(2) .
