Isolation of a Catenated Organotelluride Anion in the Sodium Borohydride Reduction of Diphenylditelluride
Witthaut, Daniel; Kirschbaum, Kristin; Conrad, Olaf; Giolando, Dean M.; Organometallics 19 (2000) 5238–; doi:10.1021/om000669e

data_4077632
_publ_section_title
;
 Isolation of a Catenated Organotelluride Anion in the Sodium Borohydride
 Reduction of Diphenylditelluride
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5238
_journal_paper_doi               10.1021/om000669e
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C42 H35 As Te3'
_chemical_formula_weight         997.42
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.285(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4734(1)
_cell_length_b                   28.8035(2)
_cell_length_c                   14.1073(1)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    180(1)
_cell_measurement_theta_max      29.01
_cell_measurement_theta_min      2.45
_cell_volume                     3730.40(6)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL and the Toledo cifomatic''
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(1)
_diffrn_measurement_device       Platform
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20541
_diffrn_reflns_theta_max         29.76
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    3.239
_exptl_absorpt_correction_T_max  0.745940
_exptl_absorpt_correction_T_min  0.560779
_exptl_absorpt_correction_type
'Empirical :Multipole Expansion (Blessing, 1995)''
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_description       chunky
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.030
_refine_ls_goodness_of_fit_obs   1.062
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         9771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_restrained_S_obs      1.062
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_obs          0.0270
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+0.2362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0604
_refine_ls_wR_factor_obs         0.0562
_reflns_number_observed          8053
_reflns_number_total             9771
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om000669e.cif
_cod_data_source_block           '[Ph4As][(TePh)3]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+0.2362P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+0.2362P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3730.39(5)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4077632