Reactions of Tris(amino)phosphines with Arylsulfonyl Azides: Product Dependency on Tris(amino)phosphine Structure
Natesan Thirupathi; Xiaodong Liu; John G. Verkade; Inorganic Chemistry 42 (2003) 389–397; doi:10.1021/ic025920s

data_4312962
_publ_section_title
;
 Reactions of Tris(amino)phosphines with Arylsulfonyl Azides: Product
 Dependency on Tris(amino)phosphine Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              389
_journal_page_last               397
_journal_paper_doi               10.1021/ic025920s
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C16 H29 N7 O3.5 P S'
_chemical_formula_weight         438.49
_chemical_name_systematic
;
  ?
;
_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                73.3363(10)
_cell_angle_beta                 84.5807(10)
_cell_angle_gamma                85.4542(10)
_cell_formula_units_Z            4
_cell_length_a                   10.7246(5)
_cell_length_b                   13.0474(6)
_cell_length_c                   15.5374(7)
_cell_measurement_temperature    173(2)
_cell_volume                     2070.40(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8403
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.270
_exptl_absorpt_correction_T_max  0.9735
_exptl_absorpt_correction_T_min  0.8770
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         8403
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                6309
_reflns_number_total             8403
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025920s_s1.cif
_cod_data_source_block           ver38
_cod_original_formula_sum        'C16 H29 N7 O3.50 P S'
_cod_database_code               4312962