Electrochemical and Chemical Oxidation of Dithia-, Diselena-, Ditellura-, Selenathia-, and Tellurathiamesocycles and Stability of the Oxidized Species
Dennis H. Evans; Nadine E. Gruhn; Jin Jin; Bo Li; Edward Lorance; Noriko Okumura; Norma A. Macías-Ruvalcaba; Uzma I. Zakai; Shao-Zhong Zhang; Eric Block; Richard S. Glass; Journal of Organic Chemistry 75 (2010) 1997–2009; doi:10.1021/jo9026484

data_4025310
_publ_section_title
;
 Electrochemical and Chemical Oxidation of Dithia-, Diselena-, Ditellura-,
 Selenathia-, and Tellurathiamesocycles and Stability of the Oxidized
 Species
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1997
_journal_page_last               2009
_journal_paper_doi               10.1021/jo9026484
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         '(Te (CH2)6 S)2 O1 (BF4)2'
_chemical_formula_sum            'C12 H24 B2 F8 O S2 Te2'
_chemical_formula_weight         677.25
_chemical_melting_point          ?
_chemical_name_systematic
; 
 5,5'-Oxy-bis(5-thiatellurocane) Bis(tetrafluoroborate 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.4920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5331(8)
_cell_length_b                   9.0124(8)
_cell_length_c                   13.0975(11)
_cell_measurement_reflns_used    5605
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.77
_cell_volume                     1060.79(16)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXCIF-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide \w exposures'
_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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9120
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    3.016
_exptl_absorpt_correction_T_max  0.7525
_exptl_absorpt_correction_T_min  0.6952
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.103
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_coef       na
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4662
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0413P)^2^+0.4797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                3943
_reflns_number_total             4662
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo9026484_si_004.cif
_cod_data_source_block           (10)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4025310