Elongated phosphoranes by C???C coupling of haloaroylmethylidenetriphenylphosphoranes: synthesis and applications
Thiemann, Thies; Umeno, Kuniharu; Wang, Jian; Tabuchi, Yumiko; Arima, Kazuya; Watanabe, Masataka; Tanaka, Yasuko; Gorohmaru, Hideki; Mataka, Shuntaro; Journal of the Chemical Society, Perkin Transactions 1  (2002) 2090–; doi:10.1039/b202745n

data_7204414
_publ_section_title
;
 Elongated phosphoranes by C???C coupling of
 haloaroylmethylidenetriphenylphosphoranes: synthesis and applications
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2090
_journal_paper_doi               10.1039/b202745n
_journal_year                    2002
_chemical_formula_moiety         'C36 H27 O P '
_chemical_formula_sum            'C36 H27 O P'
_chemical_formula_weight         506.58
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.0(5)
_cell_angle_beta                 96.1(8)
_cell_angle_gamma                90.0(6)
_cell_formula_units_Z            4
_cell_length_a                   21.492(1)
_cell_length_b                   8.0545(4)
_cell_length_c                   15.4024(9)
_cell_measurement_reflns_used    12140
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.5
_cell_volume                     2651(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows version1.06(MSC,1997-1999)'
_computing_publication_material  'teXsan for Windows version1.06(MSC,1997-1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183.2
_diffrn_measurement_device       'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w/2\q
_diffrn_orient_matrix_UB_11      0.01250
_diffrn_orient_matrix_UB_12      -0.03798
_diffrn_orient_matrix_UB_13      0.06118
_diffrn_orient_matrix_UB_21      0.04139
_diffrn_orient_matrix_UB_22      -0.03706
_diffrn_orient_matrix_UB_23      -0.01715
_diffrn_orient_matrix_UB_31      0.01790
_diffrn_orient_matrix_UB_32      0.11224
_diffrn_orient_matrix_UB_33      0.01504
_diffrn_radiation_detector       'Imaging Plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.00000
_diffrn_reflns_av_sigmaI/netI    0.1069
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6425
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.9934
_exptl_absorpt_correction_T_min  0.9492
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1064.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.36
_refine_ls_extinction_coef       0.0033(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1411
_refine_ls_R_factor_gt           0.0694
_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^)+(0.0976P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1643
_refine_ls_wR_factor_ref         0.2004
_reflns_number_gt                3186
_reflns_number_total             6007
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202745n.txt
_cod_data_source_block           '_4l'
_cod_original_cell_volume        2651(2)
_cod_original_sg_symbol_H-M      'P 21/c     '
_cod_original_formula_sum        'C36 H27 O P '
_cod_database_code               7204414