[1 + 4]-Cycloaddition of a stable silylene to 2,4,6-tri-tert-butyl-1,3,5-triphosphabenzene
Clendenning, Scott B.; Gehrhus, Barbara; Hitchcock, Peter B.; Nixon, John F.; Chemical Communications  (1999) 2451–; doi:10.1039/a908483e

data_7110746
_publ_section_title
;
 [1 + 4]-Cycloaddition of a stable silylene to
 2,4,6-tri-tert-butyl-1,3,5-triphosphabenzene
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2451
_journal_paper_doi               10.1039/a908483e
_journal_year                    1999
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C31 H53 N2 P3 Si'
_chemical_formula_structural     'C31 H53 N2 P3 SI'
_chemical_formula_sum            'C31 H53 N2 P3 Si'
_chemical_formula_weight         574.75
_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_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             1999-09-02T14:03:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                77.81(4)
_cell_angle_beta                 76.87(3)
_cell_angle_gamma                62.15(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0632(18)
_cell_length_b                   11.090(5)
_cell_length_c                   15.682(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      8.4
_cell_measurement_theta_min      7.3
_cell_measurement_wavelength     0.71073
_cell_volume                     1644.3(12)
_computing_cell_refinement       'CAD4  (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4  (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.33094E-1
_diffrn_orient_matrix_UB_12      0.53927E-1
_diffrn_orient_matrix_UB_13      -0.50896E-1
_diffrn_orient_matrix_UB_21      -0.86805E-1
_diffrn_orient_matrix_UB_22      0.31917E-1
_diffrn_orient_matrix_UB_23      -0.25283E-1
_diffrn_orient_matrix_UB_31      -0.45375E-1
_diffrn_orient_matrix_UB_32      0.81342E-1
_diffrn_orient_matrix_UB_33      0.33494E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5781
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.09
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  0.9537
_exptl_absorpt_correction_T_min  0.9316
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.054
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+3.8836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1365
_reflns_number_gt                4575
_reflns_number_total             5781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            908483esup1.cif
_cod_data_source_block           sep299
_cod_original_cell_volume        1644.4(11)
_cod_database_code               7110746
_diffrn_standards_decay_corr_max 1.049
_diffrn_standards_decay_corr_min 0.978