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_4086700
_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         'C26 H17 O5 P W'
_chemical_formula_sum            'C26 H17 O5 P W'
_chemical_formula_weight         624.22
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.21 svn.r3092 for OlexSys, GUI svn.r4949)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.753(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7996(3)
_cell_length_b                   12.5640(7)
_cell_length_c                   24.7311(12)
_cell_measurement_reflns_used    5852
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.9140
_cell_measurement_theta_min      3.6860
_cell_volume                     2395.3(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -14.00   18.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323 -107.0000  -93.0000 64

  2 omega  -49.00  -15.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  107.0000    4.0000 68

  3 omega   -6.00   20.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885 -107.0000  -93.0000 52

  4 omega  -24.00   24.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000 -180.0000 96

  5 omega  -85.00    4.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -57.0000  -60.0000 178

  6 omega   37.00   96.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  178.0000 -180.0000 118

  7 omega   39.00   95.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  178.0000   90.0000 112

  8 omega   36.00   96.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  178.0000 -150.0000 120
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0049416000
_diffrn_orient_matrix_UB_12      -0.0395802000
_diffrn_orient_matrix_UB_13      0.0201433000
_diffrn_orient_matrix_UB_21      -0.0524154000
_diffrn_orient_matrix_UB_22      -0.0317656000
_diffrn_orient_matrix_UB_23      -0.0196885000
_diffrn_orient_matrix_UB_31      0.0755196000
_diffrn_orient_matrix_UB_32      -0.0246413000
_diffrn_orient_matrix_UB_33      -0.0069854000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17483
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.923
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45129
_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    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0227P)^2^+1.1200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0590
_reflns_number_gt                4243
_reflns_number_total             4881
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00642_si_001.cif
_cod_data_source_block           201411251
_cod_depositor_comments
'Adding full bibliography for 4086699--4086700.cif.'
_cod_original_cell_volume        2395.26(19)
_cod_database_code               4086700
_chemical_oxdiff_formula         C1H1O1N4P1W1
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C21(H21), C22(H22), C24(H24), C25(H25)
2.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'