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_4346254
_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_formula_moiety         'C70  H109  Cl2  N4  P5  W2'
_chemical_formula_sum            'C70 H109 Cl2 N4 P5 W2'
_chemical_formula_weight         1600.06
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2014-09-15T10:22:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.4562(5)
_cell_length_b                   20.5506(6)
_cell_length_c                   36.1583(15)
_cell_measurement_reflns_used    10008
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.7492
_cell_measurement_theta_min      2.193
_cell_measurement_wavelength     0.71073
_cell_volume                     15200.5(9)
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'KM4, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1215
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            43530
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.1
_diffrn_reflns_theta_min         2.197
_exptl_absorpt_coefficient_mu    3.24
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies, Version 1.171.35.15
Analytical numeric absorption correction using a multifaceted crystal
        model based on expressions derived by R.C. Clark & J.S. Reid.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown-red
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6512
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.0568
_exptl_crystal_size_min          0.0444
_refine_diff_density_max         3.132
_refine_diff_density_min         -2.64
_refine_diff_density_rms         0.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     777
_refine_ls_number_reflns         13425
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1593
_refine_ls_R_factor_gt           0.0796
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1025P)^2^+105.4015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.2409
_reflns_number_gt                7421
_reflns_number_total             13425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01063_si_001.cif
_cod_data_source_block           comp_4
_cod_database_code               4346254