Blocking Intramolecular Cycloadditions between C≡C Triple Bonds and Electrophilic Phosphinidene Complexes: Generation of Intermediates Able To React with Arenes
Zhao, Xu; Lu, Zongming; Wang, Qiuyan; Wei, Donghui; Lu, Yunpeng; Duan, Zheng; Mathey, Francois; Organometallics 35 (2016) 3440–; doi:10.1021/acs.organomet.6b00642

data_4086699
_publ_section_title
;
 Blocking Intramolecular Cycloadditions between C\\tb C Triple Bonds and
 Electrophilic Phosphinidene Complexes: Generation of Intermediates Able
 To React with Arenes
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              3440
_journal_paper_doi               10.1021/acs.organomet.6b00642
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C25 H13 O5 P W'
_chemical_formula_sum            'C25 H13 O5 P W'
_chemical_formula_weight         608.17
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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_date             2015-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.930(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5740(9)
_cell_length_b                   6.6713(4)
_cell_length_c                   18.4915(7)
_cell_measurement_reflns_used    3467
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      28.1220
_cell_measurement_theta_min      3.2470
_cell_volume                     2152.13(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   32.00   88.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885   57.0000    0.0000 56

  2 omega  -39.00   88.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885    0.0000 -180.0000 127

  3 omega   58.00   92.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  178.0000    0.0000 34

  4 omega  -24.00    1.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885   19.0000  -60.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0287635000
_diffrn_orient_matrix_UB_12      -0.0151020000
_diffrn_orient_matrix_UB_13      0.0231419000
_diffrn_orient_matrix_UB_21      0.0257270000
_diffrn_orient_matrix_UB_22      -0.0606058000
_diffrn_orient_matrix_UB_23      0.0231659000
_diffrn_orient_matrix_UB_31      0.0129657000
_diffrn_orient_matrix_UB_32      0.0861629000
_diffrn_orient_matrix_UB_33      0.0203798000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9275
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         3.25
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.477
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.659
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4399
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0185P)^2^+0.1840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0578
_reflns_number_gt                3667
_reflns_number_total             4399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00642_si_003.cif
_cod_data_source_block           20150120
_cod_depositor_comments
'Adding full bibliography for 4086699--4086700.cif.'
_cod_original_cell_volume        2152.12(19)
_cod_database_code               4086699
_chemical_oxdiff_formula         C20H20N4O4W1
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 P1-H1
 0.9 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C16(H16), C17(H17), C18(H18), C19(H19),
 C22(H22), C23(H23), C24(H24), C25(H25)
;
_olex2_submission_special_instructions 'No special instructions were received'