π-Conjugated Phosphasilenes Stabilized by Fused-Ring Bulky Groups
Baolin Li; Tsukasa Matsuo; Daisuke Hashizume; Hiroyuki Fueno; Kazuyoshi Tanaka; Kohei Tamao; Journal of the American Chemical Society 131 (2009) 13222–13223; doi:10.1021/ja9051153

data_4105036
_publ_section_title
;
 \p-Conjugated Phosphasilenes Stabilized by Fused-Ring Bulky Groups
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13222
_journal_page_last               13223
_journal_paper_doi               10.1021/ja9051153
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C70 H99 P Si, C4 H8 O'
_chemical_formula_sum            'C74 H107 O P Si'
_chemical_formula_weight         1071.66
_chemical_name_systematic
; 
 (E)-1,2-bis(1,1,3,3,5,5,7,7-octaethyl-s-hydrindacen-4-yl)-
 2-(2- anthryl)phosphasilene tetrahydrofuran solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                92.9717(15)
_cell_angle_beta                 94.9680(11)
_cell_angle_gamma                101.2142(11)
_cell_formula_units_Z            2
_cell_length_a                   13.7835(3)
_cell_length_b                   14.4694(4)
_cell_length_c                   16.1200(5)
_cell_measurement_reflns_used    85604
_cell_measurement_temperature    90
_cell_measurement_theta_max      31.09
_cell_measurement_theta_min      1.51
_cell_volume                     3133.96(15)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC-8 with Saturn70 CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            69624
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.9912
_exptl_absorpt_correction_T_min  0.9307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   MULABS
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         14368
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0671
_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^)+(0.1306P)^2^+1.4346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.2117
_reflns_number_gt                10468
_reflns_number_total             14368
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja9051153_si_003.cif
_cod_data_source_block           1c-THF
_cod_database_code               4105036