
# om990768w.cif

data_global

# SUBMISSION DETAILS

_publ_contact_author_name  'Neil Burford'
_publ_contact_author_address
;
   Department of Chemistry
   Dalhousie University
   Halifax, NS B3H 4J3
   CANADA
;
_publ_contact_author_email 'burford@chem1.chem.dal.ca'
_publ_contact_author_fax   '(902) 494-1310'
_publ_contact_author_phone '(902) 494-3190'
_publ_requested_journal    'Organometallics'

# TITLE AND AUTHOR LIST

_publ_section_title
;
 Synthesis and characterization of the
 bis(2,4,6-tris[trifluoromethyl]phenyl)derivatives of arsenic and
 antimony: X-ray crystal structures of As(R~F~)~2~Cl, Sb(R~F~)~2~Cl and
 Sb(R~F~)~2~OSO~2~CF~3~
;
_publ_section_title_footnote    ?

loop_
 _publ_author_name 
 _publ_author_footnote
 _publ_author_address

 'Neil Burford'
;
 ?
;
;
   Department of Chemistry
   Dalhousie University
   Halifax, NS B3H 4J3
   CANADA
;

 'Charles L.B. Macdonald'
;
 ?
;
;
   Department of Chemistry
   Dalhousie University
   Halifax, NS B3H 4J3
   CANADA
;

 'Daren J. LeBlanc'
;
 ?
;
;
   Department of Chemistry
   Dalhousie University
   Halifax, NS B3H 4J3
   CANADA
;

 'T. Stanley Cameron'
;
 ?
;
;
   Department of Chemistry
   Dalhousie University
   Halifax, NS B3H 4J3
   CANADA
;

# TEXT

_publ_section_references
;
 Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). SIR92.
 J. Appl. Cryst., 26, 343.

 Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., de Gelder, R.,
 Israel, R. and Smits, J.M.M. (1994). DIRDIF94. The DIRDIF-94 program system,
 Technical Report of the Crystallography Laboratory, University of Nijmegen,
 The Netherlands.

 Nonius, B.V. (1997). Delft, Holland.

 Sheldrick, G.M. (1994). SHELXTL. Release 5.03. Siemens Analytical X-ray
 Instruments Inc., Madison, Wisconsin, USA.

 Sheldrick, G.M. (1997). SHELX-97. Programs for the Solution and Refinement
 of Crystal Structures. University of G\"ottingen, Germany.

 teXsan for Windows. (1997). Crystal Structure Analysis Package, Molecular
 Structure Corporation.
;

_publ_section_exptl_refinement  
;
 For 2a, all non-hydrogen atoms were refined anisotropically.  The four H 
 atoms were found and refined with a common isotropic displacement parameter 
 (FVAR 2).  The H atoms were constrained to ride on their attached carbon 
 atoms but the coordinates were allowed to vary (AFIX 44) and the C-H bond 
 distances were restrained to be equal (SADI, su = 0.02).  The C18 and C28 
 CF~3~ groups were modelled as a two-positioned disorder with their C-F 
 distances restrained to be equal (SADI, su = 0.02).  Absorption was 
 corrected for based upon the redundancy of the data (DENZO-SMN, Nonius,
 1997).  Decay was negligible.

 For 2b, 3 and 4, some non-hydrogen atoms were refined anisotropically while 
 the rest were refined isotropically.  Hydrogen atoms were included but not 
 refined.  The disordered CF~3~ groups were refined as rigid bodies riding on 
 the attached carbon atom; the fluorine anisotropic displacement parameters 
 were constrained to give a physically meaningful vibration along the C-F 
 bonds.
;

data_chuck39_2b 
 
_audit_creation_method            'manual editing' 

# CHEMICAL DATA

_chemical_name_systematic           ? 
_chemical_name_common             ? 
_chemical_melting_point           '98-100'
_chemical_formula_moiety          ? 
_chemical_formula_sum           'C18 H4 As Cl F18' 
_chemical_formula_weight          672.58 
 
# SCATTERING FACTORS

loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'F'  'F'   0.0171   0.0103 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'As'  'As'   0.0499   2.0058 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

# CRYSTAL DATA
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    'P 21/a' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z' 
 
_cell_length_a                    8.705(9) 
_cell_length_b                    30.38(1) 
_cell_length_c                    8.167(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.53(6) 
_cell_angle_gamma                 90.00 
_cell_volume                      2159(2) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(1) 
_cell_measurement_reflns_used     20 
_cell_measurement_theta_min       3.2 
_cell_measurement_theta_max       10.4 
 
_exptl_crystal_description        prism 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.40 
_exptl_crystal_size_mid           0.30 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.069 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1296 
_exptl_absorpt_coefficient_mu     1.859 
_exptl_absorpt_correction_type    'psi-scan' 
_exptl_absorpt_correction_T_min   0.615 
_exptl_absorpt_correction_T_max   1.000 
_exptl_absorpt_process_details    ? 
 
# EXPERIMENTAL DATA
 
_exptl_special_details 
; 
 ? 
; 

_diffrn_ambient_temperature       296(1) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'rotating anode (54 kV, 170 mA)' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Rigaku AFC5R' 
_diffrn_measurement_method        '\w-2\q scans' 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  50 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         2.6 
_diffrn_reflns_number             4082 
_diffrn_reflns_av_R_equivalents   0.109 
_diffrn_reflns_av_sigmaI/netI     ? 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        34 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        8 
_diffrn_reflns_theta_min          ? 
_diffrn_reflns_theta_max          25.1 
_reflns_number_total              3825 
_reflns_number_gt                 803 
_reflns_threshold_expression      I>3sigma(I) 
 
# HARDWARE/SOFTWARE

_computing_data_collection        'Rigaku AFC5R' 
_computing_cell_refinement        'Rigaku AFC5R' 
_computing_data_reduction         'Rigaku AFC5R' 
_computing_structure_solution      DIRDIF94 
_computing_structure_refinement    teXsan 
_computing_molecular_graphics     'SHELXTL (Sheldrick, 1994) and teXsan' 
_computing_publication_material   ? 
 
# REFINEMENT DATA

_refine_special_details 
; 
 ?
;
 
_refine_ls_structure_factor_coef  F  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       unit  
_refine_ls_weighting_details      ?
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     noref 
_refine_ls_extinction_method      secondary 
_refine_ls_extinction_coef        1.48764e-007 
_refine_ls_number_reflns          803 
_refine_ls_number_parameters      206 
_refine_ls_number_restraints      ? 
_refine_ls_R_factor_all           ? 
_refine_ls_R_factor_gt            0.067 
_refine_ls_wR_factor_ref          0.073 
_refine_ls_wR_factor_gt           0.073 
_refine_ls_goodness_of_fit_ref    1.73 
_refine_ls_restrained_S_all       ? 
_refine_ls_shift/su_max           0.09 
_refine_ls_shift/su_mean          ? 
 
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_B_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
As1  As  0.5360(3) -0.12252(7)  0.2545(3)  4.37(6) Uani 1    1 d . . . 
Cl1  Cl  0.6994(8) -0.1019(2)   0.0718(9)  7.5(2)  Uani 1    1 d . . . 
F1   F   0.483(2)  -0.2046(4)   0.447(2)   6.6(3)  Biso 1    1 d . . . 
F2   F   0.705(2)  -0.2073(4)   0.328(2)   7.0(4)  Biso 1    1 d . . . 
F3   F   0.570(2)  -0.2652(5)   0.354(2)   7.7(4)  Biso 1    1 d . . . 
F4   F   0.322(4)  -0.2733(9)  -0.346(4)   7.0(7)  Biso 0.50 1 d P A 1 
F5   F   0.237(3)  -0.3070(8)  -0.147(3)   5.3(6)  Biso 0.50 1 d P A 1 
F6   F   0.468(4)  -0.310(1)   -0.207(4)   8.1(8)  Biso 0.50 1 d P A 1 
F7   F   0.225(2)  -0.1249(5)  -0.224(2)  10.7(6)  Uani 1    1 d . . . 
F8   F   0.451(2)  -0.1191(4)  -0.273(2)   8.4(4)  Uani 1    1 d . . . 
F9   F   0.366(2)  -0.0870(4)  -0.063(2)   9.4(5)  Uani 1    1 d . . . 
F10  F   0.028(1)  -0.1219(4)   0.371(2)   6.7(3)  Biso 1    1 d . . . 
F11  F   0.119(1)  -0.1431(4)   0.149(2)   6.3(3)  Biso 1    1 d . . . 
F12  F   0.249(1)  -0.1507(4)   0.371(2)   6.6(3)  Biso 1    1 d . . . 
F13  F  -0.051(2)   0.0305(4)   0.346(2)   8.3(5)  Uani 1    1 d . . . 
F14  F   0.130(2)   0.0733(4)   0.294(2)   9.8(6)  Uani 1    1 d . . . 
F15  F   0.004(2)   0.0444(5)   0.098(2)   8.8(5)  Uani 1    1 d . . . 
F16  F   0.667(1)  -0.0064(4)   0.140(1)   4.9(3)  Biso 1    1 d . . . 
F17  F   0.610(1)   0.0237(4)   0.359(1)   5.1(3)  Biso 1    1 d . . . 
F18  F   0.685(1)  -0.0434(4)   0.357(1)   5.2(3)  Biso 1    1 d . . . 
F19  F   0.217(4)  -0.2795(9)  -0.276(4)   7.9(8)  Biso 0.50 1 d P A 2 
F20  F   0.454(3)  -0.2864(8)  -0.314(3)   5.0(6)  Biso 0.50 1 d P A 2 
F21  F   0.371(3)  -0.3231(8)  -0.115(3)   6.0(6)  Biso 0.50 1 d P A 2 
C1   C   0.450(2)  -0.1696(5)   0.098(2)   2.6(4)  Biso 1    1 d . . . 
C2   C   0.389(3)  -0.1664(7)  -0.061(3)   4.8(5)  Biso 1    1 d . . . 
C3   C   0.353(2)  -0.2022(7)  -0.162(3)   4.1(5)  Biso 1    1 d . . . 
C4   C   0.380(2)  -0.2439(7)  -0.096(3)   4.4(5)  Biso 1    1 d . A . 
C5   C   0.451(2)  -0.2495(7)   0.059(3)   4.1(5)  Biso 1    1 d . . . 
C6   C   0.482(2)  -0.2137(6)   0.158(3)   3.8(5)  Biso 1    1 d . . . 
C7   C   0.363(4)  -0.123(1)   -0.154(4)   7.1(7)  Biso 1    1 d . . . 
C8   C   0.347(3)  -0.2836(7)  -0.201(3)   4.1(5)  Biso 1    1 d . . . 
C9   C   0.555(3)  -0.2209(8)   0.323(3)   5.5(6)  Biso 1    1 d . . . 
C10  C   0.382(2)  -0.0729(6)   0.255(2)   3.9(5)  Biso 1    1 d . . . 
C11  C   0.223(2)  -0.0787(6)   0.261(2)   3.2(4)  Biso 1    1 d . . . 
C12  C   0.125(2)  -0.0437(6)   0.261(2)   3.0(4)  Biso 1    1 d . . . 
C13  C   0.175(2)  -0.0024(5)   0.252(2)   2.1(3)  Biso 1    1 d . . . 
C14  C   0.327(2)   0.0063(6)   0.251(2)   3.1(4)  Biso 1    1 d . . . 
C15  C   0.437(2)  -0.0289(6)   0.258(2)   3.2(4)  Biso 1    1 d . . . 
C16  C   0.157(3)  -0.1245(8)   0.287(3)   4.8(5)  Biso 1    1 d . . . 
C17  C   0.068(3)   0.0361(8)   0.250(4)   4.9(6)  Biso 1    1 d . . . 
C18  C   0.597(2)  -0.0140(5)   0.274(2)   1.9(4)  Biso 1    1 d . . . 
H1   H   0.3121    -0.1984     -0.2698     4.9584  Biso 1    1 c R . . 
H2   H   0.4777    -0.2782      0.0958     4.9414  Biso 1    1 c R . . 
H3   H   0.0182    -0.0490      0.2689     3.6062  Biso 1    1 c R . . 
H4   H   0.3621     0.0359      0.2453     3.7401  Biso 1    1 c R . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
As1  0.072(2) 0.038(1) 0.056(1) -0.009(2) -0.005(1)  0.009(2) 
Cl1  0.084(5) 0.070(4) 0.136(7) -0.025(4)  0.051(5) -0.006(4) 
F7   0.15(2)  0.09(1)  0.16(2)   0.04(1)  -0.07(1)   0.02(1)   
F8   0.18(2)  0.077(9) 0.062(9)  0.01(1)   0.04(1)   0.01(1)   
F9   0.28(2)  0.038(8) 0.044(9)  0.004(7)  0.03(1)   0.04(1)  
F13  0.11(1)  0.09(1)  0.12(1)   0.01(1)   0.01(1)   0.042(9)  
F14  0.12(1)  0.05(1)  0.20(2)  -0.05(1)  -0.04(1)   0.031(9)  
F15  0.13(1)  0.12(1)  0.08(1)   0.016(9) -0.01(1)   0.07(1)  
 
# MOLECULAR GEOMETRY

_geom_special_details 
; 
 ?
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
As1 Cl1 2.181(9) . ? 
As1 C1  2.05(2)  . ? 
As1 C10 2.02(3)  . ? 
F1  C9  1.30(3)  . ? 
F2  C9  1.37(3)  . ? 
F3  C9  1.38(3)  . ? 
F4  C8  1.24(4)  . ? 
F5  C8  1.28(4)  . ? 
F6  C8  1.32(5)  . ? 
F7  C7  1.32(4)  . ? 
F8  C7  1.26(4)  . ? 
F9  C7  1.32(4)  . ? 
F10 C16 1.33(3)  . ? 
F11 C16 1.30(3)  . ? 
F12 C16 1.31(3)  . ? 
F13 C17 1.32(3)  . ? 
F14 C17 1.30(3)  . ? 
F15 C17 1.37(3)  . ? 
F16 C18 1.29(2)  . ? 
F17 C18 1.34(2)  . ? 
F18 C18 1.35(2)  . ? 
F19 C8  1.27(4)  . ? 
F20 C8  1.33(4)  . ? 
F21 C8  1.41(4)  . ? 
C1  C2  1.39(3)  . ? 
C1  C6  1.45(3)  . ? 
C2  C3  1.39(3)  . ? 
C2  C7  1.54(4)  . ? 
C3  C4  1.40(3)  . ? 
C4  C5  1.40(3)  . ? 
C4  C8  1.51(3)  . ? 
C5  C6  1.38(3)  . ? 
C6  C9  1.49(4)  . ? 
C10 C11 1.40(3)  . ? 
C10 C15 1.42(3)  . ? 
C11 C12 1.36(3)  . ? 
C11 C16 1.52(3)  . ? 
C12 C13 1.33(3)  . ? 
C13 C14 1.36(3)  . ? 
C13 C17 1.49(4)  . ? 
C14 C15 1.43(3)  . ? 
C15 C18 1.47(3)  . ? 
C3  H1  0.98     . ?
C5  H2  1.00     . ?
C12 H3  1.01     . ?
C14 H4  0.99     . ?
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C1  As1 Cl1  90.4(7) . . ? 
C10 As1 Cl1 103.4(8) . . ? 
C10 As1 C1  107(1)   . . ? 
C2  C1  As1 131(2)   . . ? 
C6  C1  As1 112(2)   . . ? 
C2  C1  C6  116(2)   . . ? 
C1  C2  C3  125(3)   . . ? 
C1  C2  C7  125(3)   . . ? 
C3  C2  C7  111(3)   . . ? 
C4  C3  C2  117(3)   . . ? 
C3  C4  C5  122(3)   . . ? 
C3  C4  C8  118(3)   . . ? 
C5  C4  C8  120(3)   . . ? 
C6  C5  C4  121(3)   . . ? 
C5  C6  C1  120(3)   . . ? 
C1  C6  C9  121(3)   . . ? 
C5  C6  C9  119(3)   . . ? 
F8  C7  F7  104(3)   . . ? 
F7  C7  F9  107(4)   . . ? 
F7  C7  C2  107(3)   . . ? 
F8  C7  F9  111(3)   . . ? 
F8  C7  C2  112(3)   . . ? 
F9  C7  C2  116(3)   . . ? 
F4  C8  F5  111(4)   . . ? 
F4  C8  F6  104(4)   . . ? 
F4  C8  F19  52(3)   . . ? 
F4  C8  F20  57(3)   . . ? 
F4  C8  F21 136(3)   . . ? 
F4  C8  C4  112(3)   . . ? 
F5  C8  F6  106(3)   . . ? 
F19 C8  F5   64(3)   . . ? 
F5  C8  F20 139(3)   . . ? 
F5  C8  F21  57(2)   . . ? 
F5  C8  C4  112(3)   . . ? 
F19 C8  F6  138(4)   . . ? 
F6  C8  F20  51(2)   . . ? 
F6  C8  F21  52(2)   . . ? 
F6  C8  C4  111(3)   . . ? 
F19 C8  F20 108(3)   . . ? 
F19 C8  F21 116(3)   . . ? 
F19 C8  C4  110(3)   . . ? 
F20 C8  F21 101(3)   . . ? 
F20 C8  C4  109(3)   . . ? 
F21 C8  C4  112(3)   . . ? 
F1  C9  F2  110(3)   . . ? 
F1  C9  F3  106(3)   . . ? 
F1  C9  C6  117(3)   . . ? 
F2  C9  F3  101(3)   . . ? 
F2  C9  C6  111(3)   . . ? 
F3  C9  C6  110(3)   . . ? 
C11 C10 As1 124(2)   . . ? 
C15 C10 As1 119(2)   . . ? 
C11 C10 C15 117(2)   . . ? 
C12 C11 C10 121(2)   . . ? 
C10 C11 C16 120(2)   . . ? 
C12 C11 C16 118(2)   . . ? 
C13 C12 C11 122(2)   . . ? 
C12 C13 C14 120(2)   . . ? 
C12 C13 C17 123(2)   . . ? 
C14 C13 C17 117(2)   . . ? 
C13 C14 C15 120(2)   . . ? 
C10 C15 C14 119(2)   . . ? 
C10 C15 C18 128(2)   . . ? 
C14 C15 C18 114(2)   . . ? 
F11 C16 F10 106(2)   . . ? 
F12 C16 F10 106(2)   . . ? 
F10 C16 C11 110(3)   . . ? 
F11 C16 F12 109(3)   . . ? 
F11 C16 C11 111(2)   . . ? 
F12 C16 C11 114(2)   . . ? 
F14 C17 F13 106(3)   . . ? 
F13 C17 F15 105(3)   . . ? 
F13 C17 C13 113(3)   . . ? 
F14 C17 F15 104(3)   . . ? 
F14 C17 C13 115(3)   . . ? 
F15 C17 C13 113(3)   . . ? 
F16 C18 F17 104(2)   . . ? 
F16 C18 F18 106(2)   . . ? 
F16 C18 C15 117(2)   . . ? 
F17 C18 F18 105(2)   . . ? 
F17 C18 C15 112(2)   . . ? 
F18 C18 C15 111(2)   . . ? 
C2  C3  H1  121.4    . . ?
C4  C3  H1  122.0    . . ?
C4  C5  H2  120.1    . . ?
C6  C5  H2  119.2    . . ?
C11 C12 H3  119.8    . . ?
C13 C12 H3  117.9    . . ?
C13 C14 H4  118.8    . . ?
C15 C14 H4  120.7    . . ?
 
# DIFFERENCE MAP

_refine_diff_density_max     0.53
_refine_diff_density_min    -0.40 
_refine_diff_density_rms    ? 

#===END
 
