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_4346252
_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         'C35 H61 N2 P3 W'
_chemical_formula_sum            'C35 H61 N2 P3 W'
_chemical_formula_weight         786.62
_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
_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             2014-12-16
_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                   12.8151(3)
_cell_length_b                   15.8751(4)
_cell_length_c                   37.2411(9)
_cell_measurement_reflns_used    73694
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.85
_cell_measurement_theta_min      4.19
_cell_volume                     7576.4(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1861
_diffrn_reflns_av_unetI/netI     0.0848
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            29780
_diffrn_reflns_theta_full        67.49
_diffrn_reflns_theta_max         67.49
_diffrn_reflns_theta_min         2.37
_diffrn_source                   'Cu Genix 3D'
_exptl_absorpt_coefficient_mu    7.019
_exptl_absorpt_correction_T_max  0.8876
_exptl_absorpt_correction_T_min  0.1877
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;

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    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'very thin plates'
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.622
_refine_diff_density_min         -3.314
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.07
_refine_ls_R_factor_all          0.101
_refine_ls_R_factor_gt           0.0817
_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^)+(0.1756P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2251
_refine_ls_wR_factor_ref         0.2569
_reflns_number_gt                5003
_reflns_number_total             6728
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5b01063_si_001.cif
_cod_data_source_block           comp_2
_cod_database_code               4346252