[1 + 4]-Cycloadditions of silylenes to 2,4,6-tri-tert-butyl-1,3,5-triphosphabenzene
Scott B. Clendenning; Barbara Gehrhus; Peter B. Hitchcock; Daniel F. Moser; John F. Nixon; Robert West; J. Chem. Soc., Dalton Trans.  (2002) 484–490; doi:10.1039/b108020m

data_7011142
_publ_section_title
;
 [1 + 4]-Cycloadditions of silylenes to
 2,4,6-tri-tert-butyl-1,3,5-triphosphabenzene
;
_journal_issue                   4
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              484
_journal_page_last               490
_journal_paper_doi               10.1039/b108020m
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C25 H49 N2 P3 Si1'
_chemical_formula_structural     'C25 H49 N2 P3 SI'
_chemical_formula_sum            'C25 H49 N2 P3 Si'
_chemical_formula_weight         498.66
_chemical_name_common            '[SAT N2Si + P3]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2000-11-14T16:08:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 100.983(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0980(3)
_cell_length_b                   17.8562(6)
_cell_length_c                   14.7586(4)
_cell_measurement_reflns_used    10940
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     2871.11(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18478
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         3.74
_exptl_absorpt_coefficient_mu    0.264
_exptl_absorpt_correction_T_max  0.9016
_exptl_absorpt_correction_T_min  0.9016
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.59
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         6821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+3.3871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1502
_reflns_number_gt                5243
_reflns_number_total             6821
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108020m.txt
_cod_data_source_block           nov1200
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7011142