Synthesis and Characterization of Bis(2,4,6-tris(trifluoromethyl)phenyl) Derivatives of Arsenic and Antimony: X-ray Crystal Structures of As(RF)2Cl, Sb(RF)2Cl, and Sb(RF)2OSO2CF3
Neil Burford; Charles L. B. Macdonald; Daren J. LeBlanc; T. Stanley Cameron; Organometallics 19 (2000) 152–155; doi:10.1021/om990768w

data_4063197
_publ_section_title
;
 Synthesis and Characterization of
 Bis(2,4,6-tris(trifluoromethyl)phenyl) Derivatives of Arsenic and
 Antimony: X-ray Crystal Structures of As(RF)2Cl, Sb(RF)2Cl, and
 Sb(RF)2OSO2CF3
;
_journal_name_full               Organometallics
_journal_page_first              152
_journal_page_last               155
_journal_paper_doi               10.1021/om990768w
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C18 H4 Cl F18 Sb'
_chemical_formula_weight         719.41
_chemical_melting_point          112.5(5)
_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
_audit_creation_method           'manual editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.030(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.296(2)
_cell_length_b                   30.430(7)
_cell_length_c                   8.779(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(1)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      23.2
_cell_volume                     2211(1)
_computing_cell_refinement       'Rigaku AFC5R'
_computing_data_collection       'Rigaku AFC5R'
_computing_data_reduction        'Rigaku AFC5R'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1994) and teXsan'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF94
_diffrn_ambient_temperature      296(1)
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       '\w-2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode (50 kV, 160 mA)'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3953
_diffrn_reflns_theta_max         63.45
_diffrn_reflns_theta_min         2.90
_diffrn_standards_decay_%        3.6
_exptl_absorpt_coefficient_mu    12.518
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    2.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.950
_refine_ls_extinction_coef       1.04800e-008
_refine_ls_extinction_method     secondary
_refine_ls_goodness_of_fit_ref   1.00
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         1022
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          .01
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.220
_reflns_number_gt                1022
_reflns_number_total             3874
_reflns_threshold_expression     I>3sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '112-113' was changed to '112.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4063197