#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/37/2103728.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2103728
loop_
_publ_author_name
'Koutentis, P. A.'
'Haddon, R. C.'
'Oakley, R. T.'
'Cordes, A. W.'
'Brock, C. P.'
_publ_section_title
;
 Perchlorophenalenyl radical, C₁₃Cl₉: a modulated structure with
 nine threefold-symmetric molecules in the asymmetric unit
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              680
_journal_page_last               691
_journal_paper_doi               10.1107/S0108768101011193
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C13 Cl9'
_chemical_formula_sum            'C13 Cl9'
_chemical_formula_weight         475.18
_chemical_melting_point
;
160_C(dec) in air;  248_C under Ar.
;
_chemical_name_systematic
;
perchlorophenalenyl radical
;
_space_group_IT_number           160
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_audit_creation_method
;
SHELXL-97, macros written locally, and C. P. Brock
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.704(3)
_cell_length_b                   18.704(3)
_cell_length_c                   3.7792(7)
_cell_measurement_reflns_used    63143
_cell_measurement_temperature    299.0(10)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.3
_cell_volume                     1145.0(3)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT software (Nonius, 1998)'
_computing_data_reduction        'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL PC (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SIR92 (Altomare, Cascarano, Giacovazzo, Guagliardi, Burla,
Polidori & Camalli, 1994) in maXus (Mackay, Gilmore,
Edwards, Tremayne, Stewart & Shankland, 1998)
;
_diffrn_ambient_temperature      299.0(10)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full .997
_diffrn_measured_fraction_theta_max .997
_diffrn_measurement_device_type  'Nonius Kappa-CCD diffractometer'
_diffrn_measurement_method       'φ and ω scans with 1.0° steps'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .034
_diffrn_reflns_av_sigmaI/netI    .016
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            2409
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.2
_diffrn_standards_decay_%        <1.
_exptl_absorpt_coefficient_mu    1.64
_exptl_absorpt_correction_T_max  .85
_exptl_absorpt_correction_T_min  .79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
Prisms.  The a prism axis is c. The six major faces belong
to the form {1 1 -2 0}.
;
_exptl_crystal_F_000             693
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .10
_exptl_crystal_size_min          .10
_refine_diff_density_max         .36
_refine_diff_density_min         -.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   4.08
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         323
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      4.08
_refine_ls_R_factor_all          .046
_refine_ls_R_factor_gt           .045
_refine_ls_shift/su_max          .000
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.030P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .140
_reflns_number_gt                318
_reflns_number_total             323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bs0014.cif
_cod_data_source_block           pseudor3
_cod_original_sg_symbol_H-M      R3m
_cod_database_code               2103728
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Cl1 .75782(16) -.0976(3) .1796(7) .105(3) Uani d P .50 Cl
Cl2 .7673(2) -.2507(2) -.0146(12) .1085(16) Uani d P .50 Cl
Cl3 .9320(3) -.23869(17) -.1771(7) .0913(12) Uani d P .50 Cl
C01 .8507(4) -.07464(18) .0412(16) .0575(18) Uani d S 1 C
C02 .8557(7) -.1564(5) -.003(3) .055(3) Uani d P .50 C
C03 .9368(8) -.1502(4) -.044(2) .036(4) Uani d P .50 C
C04 1.0059(5) -.0734(4) .002(2) .0357(13) Uani d P .50 C
C05 1.0000 .0000 .000(3) .0271(12) Uani d S 1 C
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cl1 .0304(10) .191(7) .0706(16) .0397(16) .0102(9) .0125(19)
Cl2 .086(2) .0671(18) .0738(16) -.0352(14) .0096(17) -.0022(16)
Cl3 .160(3) .0365(13) .0721(19) .0450(16) .003(2) -.0086(12)
C01 .027(2) .092(4) .033(3) .0133(12) .0033(19) .0017(9)
C02 .043(5) .049(5) .036(3) -.006(4) .001(3) -.002(4)
C03 .042(11) .029(3) .038(3) .018(3) .002(3) .006(2)
C04 .048(3) .037(3) .028(3) .025(3) -.001(2) .003(3)
C05 .0293(18) .0293(18) .023(3) .0147(9) .000 .000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle
_geom_angle_publ_flag
C04 C01 C02 3_765 115.0(6) no
C04 C01 Cl1 3_765 134.3(4) no
C02 C01 Cl1 . 110.1(5) no
C01 C02 C03 . 119.4(5) no
C01 C02 Cl2 . 120.2(9) no
C03 C02 Cl2 . 120.4(8) no
C02 C03 C04 . 117.4(8) no
C02 C03 Cl3 . 114.0(7) no
C04 C03 Cl3 . 128.4(10) no
C03 C04 C05 . 121.1(8) no
C01 C04 C03 2_645 114.4(7) no
C01 C04 C05 2_645 124.5(6) no
C04 C05 C04 3_765 120 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cl1 C01 . 1.652(6) no
Cl2 C02 . 1.712(8) no
Cl3 C03 . 1.688(9) no
C01 C02 . 1.587(13) no
C02 C03 . 1.470(15) no
C03 C04 . 1.381(12) no
C04 C05 . 1.431(5) no
C04 C01 2_645 1.307(9) no
