1-(Diphenylphosphino)-4-(diphenylphosphinoyl)butane
Michael L. Williams; Peter C. Healy; Nicholas K. Loh; Samuel P. C. Dunstan; Graham Smith; Acta Crystallographica Section E 59 (2003) o596–o598; doi:10.1107/S1600536803006561

data_2202185
_publ_section_title
;
 1-(Diphenylphosphino)-4-(diphenylphosphinoyl)butane
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o596
_journal_page_last               o598
_journal_paper_doi               10.1107/S1600536803006561
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C28 H28 O P2'
_chemical_formula_moiety         'C28 H28 O P2'
_chemical_formula_sum            'C28 H28 O P2'
_chemical_formula_weight         442.44
_chemical_melting_point          463.5(5)
_chemical_name_common
;
1,4-bis(diphenylphosphino)butane half oxide
;
_chemical_name_systematic
;
1-(Diphenylphosphino)-4-(diphenylphosphinoyl)butane
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                102.98(2)
_cell_angle_beta                 102.23(3)
_cell_angle_gamma                100.71(2)
_cell_formula_units_Z            1
_cell_length_a                   8.927(2)
_cell_length_b                   12.514(3)
_cell_length_c                   5.802(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      17.2
_cell_measurement_theta_min      12.6
_cell_volume                     598.4(3)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Software
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure
Corporation, 1999)
;
_computing_data_reduction
;
TEXSAN for Windows (Molecular Structure Corporation, 1999).
;
_computing_molecular_graphics    'PLATON for Windows (Spek, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC-7R'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  ' graphite'
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_av_sigmaI/netI    0.038
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            3238
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.6
_diffrn_standards_decay_%        0.54
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.20
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             234
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.28
_refine_ls_goodness_of_fit_ref   0.86
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.86
_refine_ls_R_factor_all          0.069
_refine_ls_R_factor_gt           0.048
_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/[\s^2^(Fo^2^)+(0.1P)^2^+0.507P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.137
_refine_ls_wR_factor_ref         0.154
_reflns_number_gt                2133
_reflns_number_total             2752
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk6098.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '463 -- 464' was changed to
'463.5(5)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '463 -- 464' was changed to
'463.5(5)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        598.5(3)
_cod_database_code               2202185
_cod_database_fobs_code          2202185