Reactivity of Phosphanylphosphinidene Complex of Tungsten(VI) toward Phosphines: A New Method of Synthesis of catena-Polyphosphorus Ligands.
Grubba, Rafał; Ordyszewska, Anna; Kaniewska, Kinga; Ponikiewski, Łukasz; Chojnacki, Jarosław; Gudat, Dietrich; Pikies, Jerzy; Inorganic chemistry 54 (2015) 8380–8387; doi:10.1021/acs.inorgchem.5b01063

data_4346251
_publ_section_title
;
 Reactivity of Phosphanylphosphinidene Complex of Tungsten(VI) toward
 Phosphines: A New Method of Synthesis of catena-Polyphosphorus Ligands.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8380
_journal_page_last               8387
_journal_paper_doi               10.1021/acs.inorgchem.5b01063
_journal_volume                  54
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H52 Cl N2 P2 W, C12 H30 Li O6'
_chemical_formula_sum            'C44 H82 Cl Li N2 O6 P2 W'
_chemical_formula_weight         1023.3
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2015-03-02
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                84.087(3)
_cell_angle_beta                 87.718(3)
_cell_angle_gamma                84.300(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6393(4)
_cell_length_b                   12.7411(4)
_cell_length_c                   17.4160(5)
_cell_measurement_reflns_used    12738
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.5933
_cell_measurement_theta_min      2.1748
_cell_volume                     2774.69(15)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0057457
_diffrn_orient_matrix_UB_12      -0.0446844
_diffrn_orient_matrix_UB_13      0.0271574
_diffrn_orient_matrix_UB_21      0.0469147
_diffrn_orient_matrix_UB_22      0.009567
_diffrn_orient_matrix_UB_23      0.018109
_diffrn_orient_matrix_UB_31      -0.0308145
_diffrn_orient_matrix_UB_32      0.03276
_diffrn_orient_matrix_UB_33      0.024749
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18871
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    2.227
_exptl_absorpt_correction_T_max  0.689
_exptl_absorpt_correction_T_min  0.583
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.3306
_exptl_crystal_size_mid          0.2395
_exptl_crystal_size_min          0.2021
_platon_squeeze_details
;
;
_refine_diff_density_max         2.169
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     514
_refine_ls_number_reflns         10899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.049
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.3814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                9701
_reflns_number_total             10899
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5b01063_si_001.cif
_cod_data_source_block           comp_1
_cod_database_code               4346251