#------------------------------------------------------------------------------
#$Date: 2016-01-28 06:55:46 +0200 (Thu, 28 Jan 2016) $
#$Revision: 175215 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/81/7038174.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_7038174
loop_
_publ_author_name
'Gray, Paul A.'
'Carpenter, Yuen-Ying'
'Burford, Neil'
'McDonald, Robert'
_publ_section_title
;
 2-Phosphino-1,3-diphosphonium ions.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2124
_journal_page_last               2129
_journal_paper_doi               10.1039/c5dt03116h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C7 H21 P3, 2(C F3 O3 S)'
_chemical_formula_sum            'C9 H21 F6 O6 P3 S2'
_chemical_formula_weight         496.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-08-12 deposited with the CCDC.
2015-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.8691(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2969(19)
_cell_length_b                   11.4350(17)
_cell_length_c                   13.956(2)
_cell_measurement_reflns_used    6665
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.36
_cell_volume                     2008.0(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω 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  0.0150
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17498
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_T_max  0.8534
_exptl_absorpt_correction_T_min  0.7814
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0253
_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)+(0.0365P)²+0.9698P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                4323
_reflns_number_total             4636
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c5dt03116h1.cif
_cod_data_source_block           dal1091
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7038174
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
P1 P 0.13481(2) 0.46958(3) 0.38399(2) 0.01838(8) Uani 1 1 d .
P2 P 0.27719(3) 0.35509(3) 0.41499(2) 0.01910(8) Uani 1 1 d .
P3 P -0.01135(2) 0.36438(3) 0.31295(2) 0.01860(8) Uani 1 1 d .
C1 C 0.14422(11) 0.55082(12) 0.27321(10) 0.0247(3) Uani 1 1 d .
H1A H 0.0849 0.6061 0.2503 0.030 Uiso 1 1 calc R
H1B H 0.1412 0.4958 0.2185 0.030 Uiso 1 1 calc R
H1C H 0.2116 0.5938 0.2919 0.030 Uiso 1 1 calc R
C2 C -0.07771(10) 0.42269(13) 0.18909(10) 0.0253(3) Uani 1 1 d .
H2A H -0.0837 0.5078 0.1935 0.030 Uiso 1 1 calc R
H2B H -0.1489 0.3884 0.1622 0.030 Uiso 1 1 calc R
H2C H -0.0368 0.4036 0.1440 0.030 Uiso 1 1 calc R
C3 C -0.09359(11) 0.39191(13) 0.38992(10) 0.0255(3) Uani 1 1 d .
H3A H -0.0594 0.3602 0.4579 0.031 Uiso 1 1 calc R
H3B H -0.1628 0.3542 0.3595 0.031 Uiso 1 1 calc R
H3C H -0.1036 0.4764 0.3944 0.031 Uiso 1 1 calc R
C4 C -0.00197(11) 0.20861(12) 0.30295(11) 0.0247(3) Uani 1 1 d .
H4A H 0.0344 0.1756 0.3701 0.030 Uiso 1 1 calc R
H4B H 0.0384 0.1899 0.2573 0.030 Uiso 1 1 calc R
H4C H -0.0735 0.1752 0.2760 0.030 Uiso 1 1 calc R
C5 C 0.35000(11) 0.38798(13) 0.54433(10) 0.0253(3) Uani 1 1 d .
H5A H 0.3607 0.4727 0.5523 0.030 Uiso 1 1 calc R
H5B H 0.4192 0.3487 0.5636 0.030 Uiso 1 1 calc R
H5C H 0.3100 0.3606 0.5879 0.030 Uiso 1 1 calc R
C6 C 0.26066(11) 0.19956(12) 0.40364(11) 0.0271(3) Uani 1 1 d .
H6A H 0.2216 0.1793 0.3332 0.032 Uiso 1 1 calc R
H6B H 0.2208 0.1725 0.4474 0.032 Uiso 1 1 calc R
H6C H 0.3306 0.1618 0.4241 0.032 Uiso 1 1 calc R
C7 C 0.35739(11) 0.39767(14) 0.33911(11) 0.0278(3) Uani 1 1 d .
H7A H 0.3683 0.4825 0.3437 0.033 Uiso 1 1 calc R
H7B H 0.3213 0.3757 0.2684 0.033 Uiso 1 1 calc R
H7C H 0.4263 0.3580 0.3638 0.033 Uiso 1 1 calc R
S1 S 0.38384(3) 0.76454(3) 0.44530(3) 0.02425(8) Uani 1 1 d .
F1 F 0.26280(10) 0.93880(9) 0.45845(11) 0.0601(3) Uani 1 1 d .
F2 F 0.18485(8) 0.77223(10) 0.43349(10) 0.0528(3) Uani 1 1 d .
F3 F 0.29208(11) 0.81650(12) 0.57950(9) 0.0610(3) Uani 1 1 d .
O1 O 0.38153(11) 0.64280(10) 0.46971(11) 0.0471(3) Uani 1 1 d .
O2 O 0.47625(9) 0.82723(12) 0.50523(10) 0.0455(3) Uani 1 1 d .
O3 O 0.35275(10) 0.78722(12) 0.33803(9) 0.0400(3) Uani 1 1 d .
C8 C 0.27544(12) 0.82634(14) 0.48181(12) 0.0314(3) Uani 1 1 d .
S2 S 0.12552(3) 0.25972(3) 0.64313(3) 0.02231(8) Uani 1 1 d .
F4 F -0.00477(9) 0.08129(11) 0.59812(14) 0.0785(5) Uani 1 1 d .
F5 F 0.15774(10) 0.03460(10) 0.64293(15) 0.0808(5) Uani 1 1 d .
F6 F 0.08914(16) 0.09149(15) 0.75370(14) 0.0976(6) Uani 1 1 d .
O4 O 0.23256(8) 0.26946(10) 0.71098(8) 0.0339(2) Uani 1 1 d .
O5 O 0.04740(9) 0.32842(10) 0.66823(10) 0.0379(3) Uani 1 1 d .
O6 O 0.11767(10) 0.26417(12) 0.53747(8) 0.0405(3) Uani 1 1 d .
C9 C 0.08962(14) 0.10910(15) 0.66034(17) 0.0459(4) 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
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'
O O 0.0106 0.0060 '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'
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
C1 P1 P2 100.10(5)
C1 P1 P3 100.67(5)
P2 P1 P3 109.49(2)
C5 P2 C6 107.96(7)
C5 P2 C7 107.87(7)
C6 P2 C7 107.22(7)
C5 P2 P1 102.76(5)
C6 P2 P1 119.60(5)
C7 P2 P1 110.84(5)
C3 P3 C4 107.00(7)
C3 P3 C2 107.87(7)
C4 P3 C2 108.58(7)
C3 P3 P1 104.61(5)
C4 P3 P1 119.88(5)
C2 P3 P1 108.32(5)
O2 S1 O1 115.22(8)
O2 S1 O3 114.79(8)
O1 S1 O3 113.56(8)
O2 S1 C8 104.44(8)
O1 S1 C8 103.32(8)
O3 S1 C8 103.52(7)
F3 C8 F1 107.70(14)
F3 C8 F2 107.93(13)
F1 C8 F2 107.78(14)
F3 C8 S1 112.00(12)
F1 C8 S1 110.93(11)
F2 C8 S1 110.33(10)
O5 S2 O4 116.00(7)
O5 S2 O6 114.28(7)
O4 S2 O6 113.52(7)
O5 S2 C9 104.13(8)
O4 S2 C9 103.42(8)
O6 S2 C9 103.42(9)
F4 C9 F6 107.87(17)
F4 C9 F5 106.71(17)
F6 C9 F5 107.79(18)
F4 C9 S2 112.10(14)
F6 C9 S2 111.04(15)
F5 C9 S2 111.12(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
P1 C1 1.8423(14)
P1 P2 2.2262(5)
P1 P3 2.2273(5)
P2 C5 1.7907(14)
P2 C6 1.7927(15)
P2 C7 1.7961(14)
P3 C3 1.7913(13)
P3 C4 1.7943(14)
P3 C2 1.7957(14)
S1 O2 1.4347(12)
S1 O1 1.4359(12)
S1 O3 1.4418(12)
S1 C8 1.8198(15)
F1 C8 1.3239(19)
F2 C8 1.3279(18)
F3 C8 1.3135(19)
S2 O5 1.4333(11)
S2 O4 1.4364(11)
S2 O6 1.4451(12)
S2 C9 1.8238(18)
F4 C9 1.314(2)
F5 C9 1.322(2)
F6 C9 1.320(3)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C1 P1 P2 C5 124.22(7)
P3 P1 P2 C5 -130.56(5)
C1 P1 P2 C6 -116.29(7)
P3 P1 P2 C6 -11.07(6)
C1 P1 P2 C7 9.20(7)
P3 P1 P2 C7 114.42(6)
C1 P1 P3 C3 -128.22(7)
P2 P1 P3 C3 126.95(5)
C1 P1 P3 C4 111.90(7)
P2 P1 P3 C4 7.07(6)
C1 P1 P3 C2 -13.36(7)
P2 P1 P3 C2 -118.19(5)
O2 S1 C8 F3 -57.63(13)
O1 S1 C8 F3 63.24(13)
O3 S1 C8 F3 -178.11(12)
O2 S1 C8 F1 62.75(14)
O1 S1 C8 F1 -176.38(12)
O3 S1 C8 F1 -57.73(13)
O2 S1 C8 F2 -177.89(12)
O1 S1 C8 F2 -57.02(13)
O3 S1 C8 F2 61.63(13)
O5 S2 C9 F4 62.80(17)
O4 S2 C9 F4 -175.55(14)
O6 S2 C9 F4 -56.94(16)
O5 S2 C9 F6 -57.94(16)
O4 S2 C9 F6 63.72(15)
O6 S2 C9 F6 -177.68(14)
O5 S2 C9 F5 -177.90(15)
O4 S2 C9 F5 -56.24(18)
O6 S2 C9 F5 62.36(17)
