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_4105034
_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         'C62 H95 P Si'
_chemical_formula_sum            'C62 H95 P Si'
_chemical_formula_weight         899.44
_chemical_melting_point          525(3)
_chemical_name_systematic
; 
(E)-1,2-bis(1,1,3,3,5,5,7,7-octaethyl-s-hydrindacen-4-yl)-
2-phenyl-phosphasilene 
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.444(4)
_cell_angle_beta                 88.652(5)
_cell_angle_gamma                89.4746(10)
_cell_formula_units_Z            2
_cell_length_a                   12.3099(19)
_cell_length_b                   13.943(2)
_cell_length_c                   16.083(3)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.6141
_cell_measurement_theta_min      1.2664
_cell_volume                     2759.4(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57401
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.9850
_exptl_absorpt_correction_T_min  0.9484
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   numabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         16008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0653P)^2^+0.2493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1363
_reflns_number_gt                12696
_reflns_number_total             16008
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja9051153_si_001.cif
_cod_data_source_block           1a
_cod_original_cell_volume        2759.5(8)
_cod_database_code               4105034