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_4319975
_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            'C41 H64 Cl2 N6 Ni P2 S2'
_chemical_formula_weight         896.65
_chemical_name_systematic        ?
_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                 106.3120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.5918(2)
_cell_length_b                   10.60690(10)
_cell_length_c                   22.79520(10)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      2
_cell_volume                     5010.46(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.1002
_diffrn_reflns_av_sigmaI/netI    0.1376
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21473
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  0.152536
_exptl_absorpt_correction_T_min  0.063535
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1586
_refine_ls_R_factor_gt           0.0869
_refine_ls_shift/su_max          0.259
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1172P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1957
_refine_ls_wR_factor_ref         0.2303
_reflns_number_gt                4190
_reflns_number_total             7727
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001303x_2.cif
_cod_data_source_block           (t-Bu3PN3CH2SPh)2NiCl2
_cod_original_cell_volume        5010.45(7)
_cod_database_code               4319975