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_4105037
_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         'C118 H184 P2 Si2'
_chemical_formula_sum            'C118 H184 P2 Si2'
_chemical_formula_weight         1720.77
_chemical_name_systematic
;
 1,4-bis{(E)-1,2-bis(1,1,3,3,5,5,7,7-octaethyl-s-hydrindacen-4-yl)-
 phosphasileneyl}benzene
;
_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                86.5970(10)
_cell_angle_beta                 84.3280(10)
_cell_angle_gamma                68.3500(10)
_cell_formula_units_Z            1
_cell_length_a                   11.7071(2)
_cell_length_b                   15.0538(3)
_cell_length_c                   16.0803(3)
_cell_measurement_reflns_used    35018
_cell_measurement_temperature    140
_cell_measurement_theta_max      68.19
_cell_measurement_theta_min      3.16
_cell_volume                     2620.31(9)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      140
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku Raxis-RAPID'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48797
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_reflns_theta_min         3.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  0.9706
_exptl_absorpt_correction_T_min  0.8718
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   Numabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_description       plate
_exptl_crystal_F_000             950
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         9443
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+2.2938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1518
_reflns_number_gt                6818
_reflns_number_total             9443
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja9051153_si_004.cif
_cod_data_source_block           2
_cod_original_cell_volume        2620.31(8)
_cod_database_code               4105037