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_4105035
_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         'C66 H97 P Si, C7 H8'
_chemical_formula_sum            'C73 H105 P Si'
_chemical_formula_weight         1041.63
_chemical_name_systematic
; 
 (E)-1,2-bis(1,1,3,3,5,5,7,7-octaethyl-s-hydrindacen-4-yl)-2-
(2-naphtyl)phosphasilene toluene solvate
;
_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                114.210(7)
_cell_angle_beta                 90.569(4)
_cell_angle_gamma                94.770(3)
_cell_formula_units_Z            2
_cell_length_a                   11.762(4)
_cell_length_b                   16.793(6)
_cell_length_c                   17.517(6)
_cell_measurement_reflns_used    7273
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.2
_cell_measurement_theta_min      2.1
_cell_volume                     3141.0(19)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  'CrystalStruture 3.8'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_sigmaI/netI    0.1171
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21584
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.28
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  0.9918
_exptl_absorpt_correction_T_min  0.9796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         10875
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0784
_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^)+(0.1079P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1888
_refine_ls_wR_factor_ref         0.2391
_reflns_number_gt                6115
_reflns_number_total             10875
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja9051153_si_002.cif
_cod_data_source_block           1b
_cod_original_cell_volume        3141.0(18)
_cod_database_code               4105035