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_7235448
_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         'C30 H32 P2 Te2'
_chemical_formula_sum            'C30 H32 P2 Te2'
_chemical_formula_weight         709.70
_chemical_melting_point          390
_chemical_name_common            1,6-bis(diphenyltellurophosphoryl)hexane
_chemical_name_systematic        1,6-bis(diphenyltellurophosphoryl)hexane
_chemical_properties_physical
'air-sensitive, moisture-sensitive, oxygen-sensitive'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.80(2)
_cell_angle_beta                 100.66(2)
_cell_angle_gamma                102.393(18)
_cell_formula_units_Z            2
_cell_length_a                   9.513(2)
_cell_length_b                   12.852(3)
_cell_length_c                   13.247(3)
_cell_measurement_reflns_used    6769
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.6620
_cell_measurement_theta_min      3.0154
_cell_volume                     1510.4(6)
_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  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11693
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.053
_exptl_absorpt_correction_T_max  0.7762
_exptl_absorpt_correction_T_min  0.4722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis RED (Oxford Diffraction Ltd, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_recrystallization_method
'crystallization from mixture of toluene and petrolether, T = 246 K'
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.871
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0477P)^2^+1.5127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                4687
_reflns_number_total             5940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra00157e2.cif
_cod_data_source_block           LTe20
_cod_database_code               7235448