#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:49:25 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179865 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/61/7016135.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_7016135
loop_
_publ_author_name
'Dodds, Deborah L.'
'Floure, Joelle'
'Garland, Michael'
'Haddow, Mairi F.'
'Leonard, Thomas R.'
'McMullin, Claire L.'
'Orpen, A. Guy'
'Pringle, Paul G.'
_publ_section_title
;
 Diphosphanes derived from phobane and phosphatrioxa-adamantane:
 similarities, differences and anomalies.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7137
_journal_page_last               7146
_journal_paper_doi               10.1039/c1dt10335k
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C20 H32 O6.84 P2'
_chemical_formula_sum            'C20 H32 O6.84 P2'
_chemical_formula_weight         443.77
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 107.483(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.019(3)
_cell_length_b                   8.4223(19)
_cell_length_c                   20.509(5)
_cell_measurement_reflns_used    21876
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.19
_cell_measurement_theta_min      2.92
_cell_volume                     2144.9(9)
_computing_cell_refinement       'Apex II (Bruker-AXS, 2007)'
_computing_data_collection       'Apex II (Bruker-AXS, 2007)'
_computing_data_reduction
;
SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.366
_diffrn_detector_type            'Bruker-AXS SMART APEX'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      'frames, 0.3° width'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker-AXS Kappa'
_diffrn_measurement_method       'ω & φ scans'
_diffrn_measurement_specimen_support
;
glass fibre
;
_diffrn_radiation_collimation    '0.5 mm double pinhole'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71074
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20939
_diffrn_reflns_theta_full        30.19
_diffrn_reflns_theta_max         30.19
_diffrn_reflns_theta_min         2.08
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           40
_diffrn_source_power             2
_diffrn_source_size              '0.4 x 8 mm fine focus'
_diffrn_source_target            Mo
_diffrn_source_type              'Bruker-AXS KFF Mo 2K 90\% Ceramic'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  0.9759
_exptl_absorpt_correction_T_min  0.9676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2 (Sheldrick, G.M., 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       nuget
_exptl_crystal_F_000             946.4
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0396
_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)+(0.0408P)²+1.1795P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                2344
_reflns_number_total             3160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10335k.txt
_cod_data_source_block           1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7016135
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 1.03903(3) 0.29679(4) 0.20809(2) 0.02164(11) Uani 1 1 d . . .
O1 O 0.94044(7) 0.02232(11) 0.14493(5) 0.0207(2) Uani 1 1 d . . .
O2 O 0.96538(8) 0.37996(11) 0.07632(5) 0.0210(2) Uani 1 1 d . . .
O3 O 0.89269(7) 0.13191(12) 0.03496(5) 0.0212(2) Uani 1 1 d . . .
O4 O 1.13431(19) 0.3831(3) 0.22035(13) 0.0307(9) Uani 0.418(4) 1 d P . .
C1 C 1.12178(12) -0.01623(18) 0.21194(8) 0.0262(3) Uani 1 1 d . . .
H1A H 1.0974 -0.0431 0.2514 0.039 Uiso 1 1 calc R . .
H1B H 1.1935 0.0319 0.2278 0.039 Uiso 1 1 calc R . .
H1C H 1.1249 -0.1129 0.1860 0.039 Uiso 1 1 calc R . .
C2 C 1.04384(11) 0.09996(17) 0.16658(7) 0.0205(3) Uani 1 1 d . . .
C3 C 1.07684(11) 0.14290(17) 0.10322(7) 0.0216(3) Uani 1 1 d . . .
H3A H 1.1418 0.2110 0.1168 0.026 Uiso 1 1 calc R . .
H3B H 1.0951 0.0448 0.0825 0.026 Uiso 1 1 calc R . .
C4 C 0.98684(11) 0.22975(16) 0.05081(8) 0.0206(3) Uani 1 1 d . . .
C5 C 1.01090(12) 0.26263(18) -0.01507(8) 0.0250(3) Uani 1 1 d . . .
H5A H 0.9472 0.3087 -0.0481 0.037 Uiso 1 1 calc R . .
H5B H 1.0301 0.1632 -0.0334 0.037 Uiso 1 1 calc R . .
H5C H 1.0712 0.3374 -0.0067 0.037 Uiso 1 1 calc R . .
C6 C 0.76439(12) -0.00896(19) 0.07250(8) 0.0273(3) Uani 1 1 d . . .
H6A H 0.7879 -0.1094 0.0575 0.041 Uiso 1 1 calc R . .
H6B H 0.7072 0.0377 0.0348 0.041 Uiso 1 1 calc R . .
H6C H 0.7369 -0.0286 0.1113 0.041 Uiso 1 1 calc R . .
C7 C 0.85787(11) 0.10353(17) 0.09370(7) 0.0213(3) Uani 1 1 d . . .
C8 C 0.82976(11) 0.26190(17) 0.11929(8) 0.0211(3) Uani 1 1 d . . .
H8A H 0.8079 0.2449 0.1610 0.025 Uiso 1 1 calc R . .
H8B H 0.7682 0.3101 0.0841 0.025 Uiso 1 1 calc R . .
C9 C 0.92552(11) 0.37408(17) 0.13524(7) 0.0198(3) Uani 1 1 d . . .
C10 C 0.89705(12) 0.54383(17) 0.14675(8) 0.0254(3) Uani 1 1 d . . .
H10A H 0.9614 0.6105 0.1553 0.038 Uiso 1 1 calc R . .
H10B H 0.8696 0.5484 0.1863 0.038 Uiso 1 1 calc R . .
H10C H 0.8416 0.5825 0.1061 0.038 Uiso 1 1 calc R . .
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'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
O4 P1 C2 113.21(12) . . ?
O4 P1 C9 114.11(12) . . ?
C2 P1 C9 94.08(6) . . ?
O4 P1 P1 116.42(11) . 2_755 ?
C2 P1 P1 115.64(4) . 2_755 ?
C9 P1 P1 100.40(5) . 2_755 ?
C7 O1 C2 115.81(10) . . ?
C4 O2 C9 115.64(10) . . ?
C7 O3 C4 111.83(10) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C1 106.74(12) . . ?
O1 C2 C3 108.68(11) . . ?
C1 C2 C3 111.59(11) . . ?
O1 C2 P1 112.70(9) . . ?
C1 C2 P1 113.65(10) . . ?
C3 C2 P1 103.48(9) . . ?
C4 C3 C2 111.18(11) . . ?
C4 C3 H3A 109.4 . . ?
C2 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
C2 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
O2 C4 O3 110.17(10) . . ?
O2 C4 C5 106.43(11) . . ?
O3 C4 C5 107.33(11) . . ?
O2 C4 C3 111.19(11) . . ?
O3 C4 C3 108.03(11) . . ?
C5 C4 C3 113.61(12) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 C7 O1 109.89(11) . . ?
O3 C7 C6 107.25(12) . . ?
O1 C7 C6 106.02(12) . . ?
O3 C7 C8 108.36(11) . . ?
O1 C7 C8 111.83(11) . . ?
C6 C7 C8 113.36(12) . . ?
C7 C8 C9 110.70(11) . . ?
C7 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
O2 C9 C10 105.25(11) . . ?
O2 C9 C8 108.49(11) . . ?
C10 C9 C8 113.42(12) . . ?
O2 C9 P1 106.37(9) . . ?
C10 C9 P1 112.04(10) . . ?
C8 C9 P1 110.80(10) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O4 1.394(2) . ?
P1 C2 1.8732(15) . ?
P1 C9 1.8743(15) . ?
P1 P1 2.2447(9) 2_755 ?
O1 C7 1.4314(17) . ?
O1 C2 1.4413(16) . ?
O2 C4 1.4284(17) . ?
O2 C9 1.4523(16) . ?
O3 C7 1.4291(17) . ?
O3 C4 1.4309(16) . ?
C1 C2 1.512(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.529(2) . ?
C3 C4 1.519(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.502(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.500(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.518(2) . ?
C8 C9 1.5194(19) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.513(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 O1 C2 C1 -171.60(11) . . . . ?
C7 O1 C2 C3 -51.12(15) . . . . ?
C7 O1 C2 P1 62.97(13) . . . . ?
O4 P1 C2 O1 -171.33(14) . . . . ?
C9 P1 C2 O1 -52.89(10) . . . . ?
P1 P1 C2 O1 50.70(11) 2_755 . . . ?
O4 P1 C2 C1 67.08(16) . . . . ?
C9 P1 C2 C1 -174.49(10) . . . . ?
P1 P1 C2 C1 -70.90(11) 2_755 . . . ?
O4 P1 C2 C3 -54.12(15) . . . . ?
C9 P1 C2 C3 64.31(9) . . . . ?
P1 P1 C2 C3 167.90(7) 2_755 . . . ?
O1 C2 C3 C4 50.17(15) . . . . ?
C1 C2 C3 C4 167.60(12) . . . . ?
P1 C2 C3 C4 -69.82(12) . . . . ?
C9 O2 C4 O3 55.80(15) . . . . ?
C9 O2 C4 C5 171.85(11) . . . . ?
C9 O2 C4 C3 -63.94(14) . . . . ?
C7 O3 C4 O2 -60.02(14) . . . . ?
C7 O3 C4 C5 -175.51(11) . . . . ?
C7 O3 C4 C3 61.62(14) . . . . ?
C2 C3 C4 O2 64.95(14) . . . . ?
C2 C3 C4 O3 -56.06(14) . . . . ?
C2 C3 C4 C5 -175.01(12) . . . . ?
C4 O3 C7 O1 -61.14(14) . . . . ?
C4 O3 C7 C6 -175.96(11) . . . . ?
C4 O3 C7 C8 61.32(13) . . . . ?
C2 O1 C7 O3 56.46(15) . . . . ?
C2 O1 C7 C6 172.05(11) . . . . ?
C2 O1 C7 C8 -63.93(14) . . . . ?
O3 C7 C8 C9 -57.16(14) . . . . ?
O1 C7 C8 C9 64.12(15) . . . . ?
C6 C7 C8 C9 -176.09(12) . . . . ?
C4 O2 C9 C10 -173.51(11) . . . . ?
C4 O2 C9 C8 -51.79(14) . . . . ?
C4 O2 C9 P1 67.45(12) . . . . ?
C7 C8 C9 O2 51.40(14) . . . . ?
C7 C8 C9 C10 167.97(12) . . . . ?
C7 C8 C9 P1 -65.02(13) . . . . ?
O4 P1 C9 O2 54.87(15) . . . . ?
C2 P1 C9 O2 -62.82(9) . . . . ?
P1 P1 C9 O2 -179.83(7) 2_755 . . . ?
O4 P1 C9 C10 -59.63(16) . . . . ?
C2 P1 C9 C10 -177.32(10) . . . . ?
P1 P1 C9 C10 65.67(10) 2_755 . . . ?
O4 P1 C9 C8 172.60(14) . . . . ?
C2 P1 C9 C8 54.90(10) . . . . ?
P1 P1 C9 C8 -62.11(10) 2_755 . . . ?
