Contrasting Formation of a (Phenylthio)phosphinimine and (Phenylthio)phosphazide. Synthesis of Metal Complexes
Luc LePichon; Douglas W. Stephan; Inorganic Chemistry 40 (2001) 3827–3829; doi:10.1021/ic001303x

data_4319976
_publ_section_title
;
 Contrasting Formation of a (Phenylthio)phosphinimine and
 (Phenylthio)phosphazide. Synthesis of Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3827
_journal_page_last               3829
_journal_paper_doi               10.1021/ic001303x
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C38 H67 Cl2 Fe N6 P2 S2'
_chemical_formula_weight         860.79
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.821(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.917(5)
_cell_length_b                   21.409(7)
_cell_length_c                   15.513(5)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      2.0
_cell_volume                     4612(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18168
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.152641
_exptl_absorpt_correction_T_min  0.029506
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.564
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.564
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.594
_refine_ls_shift/su_mean         0.041
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1949P)^2^+11.4083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1734
_reflns_number_gt                6185
_reflns_number_total             7932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001303x_3.cif
_cod_data_source_block           (t-Bu3PN3CH2SPh)2FeCl2
_cod_database_code               4319976