Unprecedented Ring Transformation of an α,α′-Monosubstituted 2,4,5-Triphenylpyrylium Salt with η3-Phosphines: Efficient Synthesis of Aryl- and Alkylphosphonium Triphenylcyclopentadienylides
Xu, Tao; Gong, Wei-tao; Ye, Jun-wei; Lin, Yuan; Ning, Gui-ling; Organometallics 29 (2010) 6744–; doi:10.1021/om100872f

data_4067171
_publ_section_title
;
 Unprecedented Ring Transformation of an \a,\a&#x2032;-Monosubstituted
 2,4,5-Triphenylpyrylium Salt with \h3-Phosphines: Efficient Synthesis of
 Aryl- and Alkylphosphonium Triphenylcyclopentadienylides
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6744
_journal_paper_doi               10.1021/om100872f
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C26 H26 Cl O4 P'
_chemical_formula_weight         468.89
_chemical_name_systematic
; 
 Trimethyl(2,3,5-triphenylcyclopentadienyl)phosphonium perchlorate 
;
_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                 125.869(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.352(4)
_cell_length_b                   10.2322(17)
_cell_length_c                   20.664(6)
_cell_measurement_reflns_used    12945
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.01
_cell_volume                     4686.5(17)
_computing_cell_refinement       'SMART (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXP97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_detector_area_resol_mean 'Bruker SMART CCD area'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12945
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  0.9618
_exptl_absorpt_correction_T_min  0.9495
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS; Sheldrick, (1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blcok
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         5310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.107
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0035P)^2^+10.2330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                4166
_reflns_number_total             5310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100872f_si_002.cif
_cod_data_source_block           4a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               4067171