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_4319974
_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            'C16 H28 Cl2 Fe N P S'
_chemical_formula_weight         424.17
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.1040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.32850(10)
_cell_length_b                   15.2783(3)
_cell_length_c                   15.0720(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2
_cell_volume                     2100.36(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10694
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  0.152488
_exptl_absorpt_correction_T_min  0.070517
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0493P)^2^+1.4976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1225
_reflns_number_gt                3452
_reflns_number_total             3675
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001303x_1.cif
_cod_data_source_block           '[i-Pr3PNCH2SPh)FeCl(m-Cl)]2'
_cod_original_cell_volume        2100.36(5)
_cod_database_code               4319974