#------------------------------------------------------------------------------
#$Date: 2016-05-06 04:30:11 +0300 (Fri, 06 May 2016) $
#$Revision: 182705 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/88/7038830.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_7038830
loop_
_publ_author_name
'Kirst, Christin'
'Bode, Bela E.'
'Cordes, David B.'
'Nejman, Phillip S.'
'Slawin, Alexandra M. Z.'
'Karaghiosoff, Konstantin'
'Woollins, J. Derek'
_publ_section_title
;
 Diphosphane 2,2'-binaphtho[1,8-de][1,3,2]dithiaphosphinine and the easy
 formation of a stable phosphorus radical cation.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6348
_journal_page_last               6351
_journal_paper_doi               10.1039/c6dt00304d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C20 H12 P2 S4'
_chemical_formula_sum            'C20 H12 P2 S4'
_chemical_formula_weight         442.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-02
_audit_creation_method           'by CrystalStructure 4.1'
_audit_update_record
;
2015-12-02 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                100.330(18)
_cell_angle_beta                 112.832(12)
_cell_angle_gamma                105.952(16)
_cell_formula_units_Z            1
_cell_length_a                   7.5926(8)
_cell_length_b                   7.7769(11)
_cell_length_c                   9.5253(19)
_cell_measurement_reflns_used    1633
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.50
_cell_volume                     471.75(16)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7771
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.376
_diffrn_reflns_theta_min         2.451
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             226.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.25
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1727
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0638P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1087
_reflns_number_gt                1538
_reflns_number_total             1727
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c6dt00304d2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7038829--7038830.cif.'
_cod_database_code               7038830
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
S1 S 0.37489(9) 0.04112(8) 0.64037(7) 0.0312(2) Uani 1 1 d . .
S9 S 0.07771(9) 0.09752(8) 0.79216(6) 0.0321(2) Uani 1 1 d . .
P1 P 0.06432(9) -0.07129(8) 0.58784(7) 0.0281(2) Uani 1 1 d . .
C1 C 0.4479(3) 0.2893(3) 0.6911(2) 0.0228(5) Uani 1 1 d . .
C2 C 0.6059(3) 0.3737(3) 0.6578(3) 0.0304(5) Uani 1 1 d . .
H2 H 0.6552 0.2967 0.6061 0.036 Uiso 1 1 calc R U
C3 C 0.6950(4) 0.5705(4) 0.6985(3) 0.0346(6) Uani 1 1 d . .
H3 H 0.8070 0.6258 0.6782 0.042 Uiso 1 1 calc R U
C4 C 0.6210(3) 0.6819(3) 0.7671(3) 0.0315(5) Uani 1 1 d . .
H4 H 0.6794 0.8150 0.7919 0.038 Uiso 1 1 calc R U
C5 C 0.4578(3) 0.6020(3) 0.8021(2) 0.0252(5) Uani 1 1 d . .
C6 C 0.3866(4) 0.7232(3) 0.8752(3) 0.0314(5) Uani 1 1 d . .
H6 H 0.4489 0.8558 0.8994 0.038 Uiso 1 1 calc R U
C7 C 0.2310(4) 0.6534(4) 0.9113(3) 0.0354(6) Uani 1 1 d . .
H7 H 0.1852 0.7366 0.9607 0.042 Uiso 1 1 calc R U
C8 C 0.1387(3) 0.4590(3) 0.8755(3) 0.0306(5) Uani 1 1 d . .
H8 H 0.0270 0.4109 0.8982 0.037 Uiso 1 1 calc R U
C9 C 0.2048(3) 0.3354(3) 0.8084(2) 0.0237(5) Uani 1 1 d . .
C10 C 0.3674(3) 0.4023(3) 0.7666(2) 0.0220(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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
P P 0.1023 0.0942
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(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_3
C1 S1 P1 106.53(8) .
C9 S9 P1 105.74(8) .
S1 P1 S9 99.71(4) .
S1 P1 P1 99.52(4) 2_556
S9 P1 P1 99.48(4) 2_556
C2 C1 C10 120.5(2) .
C2 C1 S1 112.55(16) .
C10 C1 S1 126.90(16) .
C1 C2 C3 121.5(2) .
C1 C2 H2 119.3 .
C3 C2 H2 119.3 .
C4 C3 C2 119.9(2) .
C4 C3 H3 120.1 .
C2 C3 H3 120.1 .
C3 C4 C5 120.7(2) .
C3 C4 H4 119.6 .
C5 C4 H4 119.6 .
C6 C5 C4 119.0(2) .
C6 C5 C10 120.1(2) .
C4 C5 C10 120.9(2) .
C7 C6 C5 121.1(2) .
C7 C6 H6 119.4 .
C5 C6 H6 119.4 .
C6 C7 C8 119.7(2) .
C6 C7 H7 120.2 .
C8 C7 H7 120.2 .
C9 C8 C7 121.7(2) .
C9 C8 H8 119.2 .
C7 C8 H8 119.2 .
C8 C9 C10 120.7(2) .
C8 C9 S9 112.78(17) .
C10 C9 S9 126.44(17) .
C5 C10 C9 116.64(19) .
C5 C10 C1 116.51(19) .
C9 C10 C1 126.84(19) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 C1 1.771(2) .
S1 P1 2.0903(9) .
S9 C9 1.782(2) .
S9 P1 2.0924(10) .
P1 P1 2.2307(12) 2_556
C1 C2 1.382(3) .
C1 C10 1.439(3) .
C2 C3 1.402(3) .
C2 H2 0.9500 .
C3 C4 1.358(4) .
C3 H3 0.9500 .
C4 C5 1.416(3) .
C4 H4 0.9500 .
C5 C6 1.415(3) .
C5 C10 1.430(3) .
C6 C7 1.355(4) .
C6 H6 0.9500 .
C7 C8 1.393(3) .
C7 H7 0.9500 .
C8 C9 1.371(3) .
C8 H8 0.9500 .
C9 C10 1.434(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
P1 S1 C1 C2 -152.29(15)
P1 S1 C1 C10 30.86(19)
C10 C1 C2 C3 1.2(3)
S1 C1 C2 C3 -175.90(18)
C1 C2 C3 C4 -2.4(4)
C2 C3 C4 C5 1.7(3)
C3 C4 C5 C6 179.3(2)
C3 C4 C5 C10 0.2(3)
C4 C5 C6 C7 -179.9(2)
C10 C5 C6 C7 -0.8(3)
C5 C6 C7 C8 -0.2(3)
C6 C7 C8 C9 1.9(3)
C7 C8 C9 C10 -2.5(3)
C7 C8 C9 S9 174.47(18)
P1 S9 C9 C8 148.74(14)
P1 S9 C9 C10 -34.48(19)
C6 C5 C10 C9 0.1(3)
C4 C5 C10 C9 179.23(19)
C6 C5 C10 C1 179.53(18)
C4 C5 C10 C1 -1.4(3)
C8 C9 C10 C5 1.5(3)
S9 C9 C10 C5 -175.08(15)
C8 C9 C10 C1 -177.9(2)
S9 C9 C10 C1 5.6(3)
C2 C1 C10 C5 0.7(3)
S1 C1 C10 C5 177.31(15)
C2 C1 C10 C9 -180.0(2)
S1 C1 C10 C9 -3.4(3)
