[4+2] Cycloaddition of 9-Anthryldiphosphene with Electron-Deficient Olefins: Transformation of a Diaryldiphosphene to Alkylaryldiphosphenes
Tsurusaki, Akihiro; Sasamori, Takahiro; Tokitoh, Norihiro; Organometallics 28 (2009) 3604–; doi:10.1021/om900284p

data_4069569
_publ_section_title
;
 [4+2] Cycloaddition of 9-Anthryldiphosphene with Electron-Deficient
 Olefins: Transformation of a Diaryldiphosphene to Alkylaryldiphosphenes
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3604
_journal_paper_doi               10.1021/om900284p
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C48 H78 N2 P2 Si7, 1.5(C6 H6)'
_chemical_formula_sum            'C57 H87 N2 P2 Si7'
_chemical_formula_weight         1058.86
_chemical_name_common            compound4d
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.025(11)
_cell_angle_beta                 79.207(11)
_cell_angle_gamma                88.701(11)
_cell_formula_units_Z            2
_cell_length_a                   11.804(5)
_cell_length_b                   12.676(6)
_cell_length_c                   22.115(9)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      3.00
_cell_volume                     3123(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  Rigaku_Mercury_CCD
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0858
_diffrn_reflns_av_sigmaI/netI    0.1355
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27384
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  0.9765
_exptl_absorpt_correction_T_min  0.9537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1142
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         11509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0747
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+1.8181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1504
_reflns_number_gt                6996
_reflns_number_total             11509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900284p_si_002.cif
_cod_data_source_block           compound4d
_cod_database_code               4069569