Redox Chemistry of Tellurium Bis(tert-butylamido)cyclodiphosph(V)azane Disulfide and Diselenide Systems: A Spectroscopic and Structural Study
Glen G. Briand; Tristram Chivers; Gabriele Schatte; Inorganic Chemistry 41 (2002) 1958–1965; doi:10.1021/ic011151l

data_4317815
_publ_contact_author_address
; Department of Chemistry
   University of Calgary
   Calgary Alberta T2N 1N4
   Canada
;
_publ_contact_author_email       chivers@ucalgary.ca
_publ_contact_author_fax         '001 403 289 9488'
_publ_contact_author_name        'Dr Tristram Chivers'
_publ_contact_author_phone       '001 403 220 5741'
_publ_section_title
;
 Redox Chemistry of Tellurium Bis(tert-butylamido)cyclodiphosph(V)azane
 Disulfide and Diselenide Systems: A Spectroscopic and Structural Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1958
_journal_page_last               1965
_journal_paper_doi               10.1021/ic011151l
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C32 H74 N8 P4 Se4 Te, C3H7'
_chemical_formula_sum            'C35 H81 N8 P4 Se4 Te'
_chemical_formula_weight         1181.40
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.554(2)
_cell_length_b                   26.697(4)
_cell_length_c                   14.2637(19)
_cell_measurement_reflns_used    4147
_cell_measurement_temperature    193(2)
_cell_volume                     5922.9(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  WinGX-1.63
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0921
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27250
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.096
_exptl_absorpt_correction_T_max  0.8606
_exptl_absorpt_correction_T_min  0.2760
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS, V 2.01, Software for Area-Detector Absorption
   Corrections; Bruker AXS Inc., Madison, WI, 2000.
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2380
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.195
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         5171
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+28.6245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1721
_reflns_number_gt                3465
_reflns_number_total             5171
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011151l_1.cif
_cod_data_source_block           6b
_cod_original_cell_volume        5923.0(14)
_cod_database_code               4317815