Successful oxidation of Ph2P(CH2)nPPh2 (n = 2, 4, 6) by tellurium leading to Ph2P(Te)(CH2)nP(Te)Ph2
Jeremias, Lukáš; Babiak, Michal; Kubát, Václav; Calhorda, Maria José; Trávníček, Zdeněk; Novosad, Josef; RSC Advances 4 (2014) 15428–; doi:10.1039/c4ra00157e

data_7235449
_publ_section_title
;
 Successful oxidation of Ph2P(CH2)nPPh2 (n = 2, 4, 6) by tellurium leading
 to Ph2P(Te)(CH2)nP(Te)Ph2
;
_journal_issue                   30
_journal_name_full               'RSC Advances'
_journal_page_first              15428
_journal_paper_doi               10.1039/c4ra00157e
_journal_volume                  4
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C28 H28 P2 Te'
_chemical_formula_sum            'C28 H28 P2 Te'
_chemical_formula_weight         554.04
_chemical_melting_point          373
_chemical_name_common
1-(diphenyltellurophosphoryl)-4-(diphenylphosphino)butane
_chemical_name_systematic
1-(diphenyltellurophosphoryl)-4-(diphenylphosphino)butane
_chemical_properties_physical
'air-sensitive, moisture-sensitive, oxygen-sensitive'
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.562(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.0157(4)
_cell_length_b                   14.2910(7)
_cell_length_c                   9.7134(4)
_cell_measurement_reflns_used    6388
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.7829
_cell_measurement_theta_min      2.8410
_cell_volume                     1230.30(10)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction Ltd, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction Ltd, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction Ltd, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.4353
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, 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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8099
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.85
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.352
_exptl_absorpt_correction_T_max  0.6489
_exptl_absorpt_correction_T_min  0.6138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis RED (Oxford Diffraction Ltd, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_recrystallization_method
'crystallization from mixture of toluene and petrolether, T = 246 K'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.545(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3937
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0569
_reflns_number_gt                3788
_reflns_number_total             3937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra00157e2.cif
_cod_data_source_block           LTe25
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7235449