Insertion of phosphinidene complexes into the P-H bond of secondary phosphine oxides: a new version of the phospha-Wittig synthesis of P[double bond, length as m-dash]C double bonds.
Hao, Yanwei; Wu, Di; Tian, Rongqiang; Duan, Zheng; Mathey, François; Dalton transactions (Cambridge, England : 2003) 45 (2016) 891–893; doi:10.1039/c5dt04245c

data_7037649
_publ_section_title
;
 Insertion of phosphinidene complexes into the P-H bond of secondary
 phosphine oxides: a new version of the phospha-Wittig synthesis of
 P[double bond, length as m-dash]C double bonds.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              891
_journal_page_last               893
_journal_paper_doi               10.1039/c5dt04245c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C23 H16 O6 P2 W, C H2 Cl2'
_chemical_formula_sum            'C24 H18 Cl2 O6 P2 W'
_chemical_formula_weight         719.07
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2015-01-26 deposited with the CCDC.
2015-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.974(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.34581(18)
_cell_length_b                   19.8000(6)
_cell_length_c                   21.5196(6)
_cell_measurement_reflns_used    4059
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.6910
_cell_measurement_theta_min      3.5300
_cell_volume                     2677.73(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -11.00   20.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2885  -99.0000 -180.0000 31

  2 omega   -2.00   82.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8666   77.0000   60.0000 84

  3 omega  -50.00   49.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8666  -77.0000  -60.0000 99

  4 omega   32.00   57.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8666 -178.0000 -180.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0937060000
_diffrn_orient_matrix_UB_12      0.0198367000
_diffrn_orient_matrix_UB_13      -0.0059743000
_diffrn_orient_matrix_UB_21      0.0486219000
_diffrn_orient_matrix_UB_22      0.0202275000
_diffrn_orient_matrix_UB_23      -0.0211978000
_diffrn_orient_matrix_UB_31      -0.0398732000
_diffrn_orient_matrix_UB_32      -0.0219611000
_diffrn_orient_matrix_UB_33      -0.0249367000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11802
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.05
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.469
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+0.1349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0720
_reflns_number_gt                4518
_reflns_number_total             5457
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04245c4.cif
_cod_data_source_block           201412270
_cod_depositor_comments          'Adding full bibliography for 7037649.cif.'
_cod_original_cell_volume        2677.73(13)
_cod_database_code               7037649
_chemical_oxdiff_formula         C20H20N4O4W1P1
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
;
_olex2_submission_special_instructions 'No special instructions were received'