Pyramidal Inversion Isomers in the Solid-State Structure of the Tricyclic Antimony-Tellurium Imido Complex TeSb2Cl2(NtBu)4
Tristram Chivers; Gabriele Schatte; Inorganic Chemistry 41 (2002) 1002–1006; doi:10.1021/ic0109694

data_4317587
_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
;
 Pyramidal Inversion Isomers in the Solid-State Structure of the Tricyclic
 Antimony-Tellurium Imido Complex TeSb2Cl2(NtBu)4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1002
_journal_page_last               1006
_journal_paper_doi               10.1021/ic0109694
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C16 H36 Cl N4 Sb2 Te, Cl'
_chemical_formula_sum            'C16 H36 Cl2 N4 Sb2 Te'
_chemical_formula_weight         726.49
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 109.385(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.150(2)
_cell_length_b                   9.4959(14)
_cell_length_c                   17.035(2)
_cell_measurement_reflns_used    6112
_cell_measurement_temperature    193(2)
_cell_volume                     2464.4(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'ORTEP-3 for WindowsNT'
_computing_publication_material  WinGX-1.62
_computing_structure_refinement  'SHELXL-97.2 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13576
_diffrn_reflns_theta_full        25.81
_diffrn_reflns_theta_max         25.81
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        '< 0.1'
_diffrn_standards_number
;
  Recollection of the first 50 phi-scan frames at the
  end of the data collection.
;
_exptl_absorpt_coefficient_mu    3.578
_exptl_absorpt_correction_T_max  0.8140
_exptl_absorpt_correction_T_min  0.3287
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; SADABS, V 5.0, Software for Area-Detector Absorption
   Corrections; Bruker AXS Inc., Madison, WI, 1998.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.872
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4692
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+3.0380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                4180
_reflns_number_total             4692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0109694_2.cif
_cod_data_source_block           3
_cod_original_cell_volume        2464.2(6)
_cod_database_code               4317587