##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in          #
# Acta Crystallographica Section E. It conforms to the requirements of       #
# Notes for Authors for Acta Crystallographica Section E, and has been       #
# peer reviewed under the auspices of the IUCr Commission on Journals.       #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic.                                       #
#                                                                            #
# Software is freely available for graphical display of the structure(s)     #
# in this CIF. For information consult the CIF software page                 #
# http://www.iucr.org/resources/cif/software.                                #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the journal # 
# article from which it was obtained.                                        #
#                                                                            #
##############################################################################
data_global
_audit_creation_method     'WinGX routine CIF_UPDATE'
_audit_conform_dict_name     cif_core.dic
_audit_conform_dict_version     2.2
_journal_date_recd_electronic     2012-07-10
_journal_date_accepted     2012-07-21
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2012
_journal_volume     68
_journal_issue      8
_journal_page_first     i67
_journal_page_last     i67
_journal_paper_category     QI
_journal_paper_doi     10.1107/S1600536812033132
_journal_coeditor_code     RU2039
_publ_contact_author
;
Dr. Oksana Sologub
National Institute for Materials Science
Namiki 1-1
Tsukuba
305-0044, Japan
;
_publ_contact_author_email     solohub.oksana@nims.go.jp
_publ_contact_author_phone     +81-29-860-8027
_publ_section_title
;
Boron carbide, B₁₃₋ₓC₂₋y (x = 0.12, y =
0.01)
;
loop_
    _publ_author_name
    _publ_author_address
    'Oksana Sologub'
;
National Institute for Materials Science
Namiki 1-1
305-0044 Tsukuba
Japan
;
    'Yuichi Michiue'
;
National Institute for Materials Science
Namiki 1-1
305-0044 Tsukuba
Japan
;
    'Takao Mori'
;
National Institute for Materials Science
Namiki 1-1
305-0044 Tsukuba
Japan
;
data_I
_chemical_name_systematic
;
Boron carbide
;
_chemical_formula_moiety     'C1.99 B12.88'
_chemical_formula_sum     'C1.99 B12.88'
_chemical_formula_iupac     'C1.99 B12.88'
_chemical_formula_weight     163.137
_symmetry_cell_setting     trigonal
_symmetry_space_group_name_H-M     'R -3 m'
_symmetry_space_group_name_Hall     '-R 3 2"'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-y, x-y, z'
    'y, x, -z'
    '-x+y, -x, z'
    '-x, -x+y, -z'
    'x-y, -y, -z'
    'x+2/3, y+1/3, z+1/3'
    '-y+2/3, x-y+1/3, z+1/3'
    'y+2/3, x+1/3, -z+1/3'
    '-x+y+2/3, -x+1/3, z+1/3'
    '-x+2/3, -x+y+1/3, -z+1/3'
    'x-y+2/3, -y+1/3, -z+1/3'
    'x+1/3, y+2/3, z+2/3'
    '-y+1/3, x-y+2/3, z+2/3'
    'y+1/3, x+2/3, -z+2/3'
    '-x+y+1/3, -x+2/3, z+2/3'
    '-x+1/3, -x+y+2/3, -z+2/3'
    'x-y+1/3, -y+2/3, -z+2/3'
    '-x, -y, -z'
    'y, -x+y, -z'
    '-y, -x, z'
    'x-y, x, -z'
    'x, x-y, z'
    '-x+y, y, z'
    '-x+2/3, -y+1/3, -z+1/3'
    'y+2/3, -x+y+1/3, -z+1/3'
    '-y+2/3, -x+1/3, z+1/3'
    'x-y+2/3, x+1/3, -z+1/3'
    'x+2/3, x-y+1/3, z+1/3'
    '-x+y+2/3, y+1/3, z+1/3'
    '-x+1/3, -y+2/3, -z+2/3'
    'y+1/3, -x+y+2/3, -z+2/3'
    '-y+1/3, -x+2/3, z+2/3'
    'x-y+1/3, x+2/3, -z+2/3'
    'x+1/3, x-y+2/3, z+2/3'
    '-x+y+1/3, y+2/3, z+2/3'
_cell_length_a     5.6530(8)
_cell_length_b     5.6530(8)
_cell_length_c     12.156(4)
_cell_angle_alpha     90
_cell_angle_beta     90
_cell_angle_gamma     120
_cell_volume     336.42(17)
_cell_formula_units_Z     3
_cell_measurement_reflns_used     20
_cell_measurement_theta_min     8
_cell_measurement_theta_max     50
_cell_measurement_temperature     293
_exptl_crystal_description     prism
_exptl_crystal_colour     black
_exptl_crystal_size_max     0.45
_exptl_crystal_size_mid     0.3
_exptl_crystal_size_min     0.21
_exptl_crystal_size_rad     ?
_exptl_crystal_density_diffrn     2.416
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     229
_exptl_absorpt_coefficient_mu     0.097
_exptl_absorpt_correction_type     none
_diffrn_ambient_temperature     293
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type     'Rigaku AFC 7R'
_diffrn_measurement_method     ω-2θ
_diffrn_reflns_number     1489
_diffrn_reflns_av_R_equivalents     0.1508
_diffrn_reflns_theta_min     4.49
_diffrn_reflns_theta_max     39.83
_diffrn_reflns_theta_full     39.83
_diffrn_measured_fraction_theta_max     1
_diffrn_measured_fraction_theta_full     1
_diffrn_reflns_limit_h_min     -10
_diffrn_reflns_limit_h_max     8
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     10
_diffrn_reflns_limit_l_min     -21
_diffrn_reflns_limit_l_max     21
_diffrn_standards_number     3
_diffrn_standards_interval_count     150
_diffrn_standards_interval_time     105
_diffrn_standards_decay_%     0
_refine_special_details
;
Refinement of F² against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F², conventional
R-factors R are based on F, with F set to zero for
negative F². The threshold expression of F² >
σ(F²) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F² are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger.
;
_reflns_number_total     284
_reflns_number_gt     184
_reflns_threshold_expression     I>2sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_gt     0.0455
_refine_ls_wR_factor_ref     0.1087
_refine_ls_goodness_of_fit_ref     1.031
_refine_ls_restrained_S_all     1.029
_refine_ls_number_reflns     284
_refine_ls_number_parameters     22
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment     noref
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0481P)²+0.3407P] where P=(Fo²+2Fc²)/3'
_refine_ls_shift/su_max     0.002
_refine_diff_density_max     0.554
_refine_diff_density_min     -0.374
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'
    B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection
                     'Rigaku/AFC Diffractometer Control Software (Rigaku, 1998)'
_computing_cell_refinement
                     'Rigaku/AFC Diffractometer Control Software (Rigaku, 1998)'
_computing_data_reduction     'TEXSAN (Molecular Structure Corporation, 1998)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'ATOMS (Dowty, 1999)'
_computing_publication_material
                  'SHELXL97 (Sheldrick, 2008) and WinGX (Farrugia, 1999)'
loop_
    _atom_site_type_symbol
    _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_occupancy
    B B1 0.44092(16) 0.55908(16) 0.05298(12) 0.0053(3) Uani 0.958(4)
    C C11 0.44092(16) 0.55908(16) 0.05298(12) 0.0053(3) Uani 0.042(4)
    B B2 0.50336(16) 0.49664(16) 0.19232(11) 0.0054(3) Uani 1
    B B3 0 0 0 0.0118(8) Uani 0.87
    C C1 0 0 0.1177(5) 0.0071(8) Uani 0.87(2)
    B B11 0 0 0.079(4) 0.0071(8) Uani 0.13(2)
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
    B1 0.0056(4) 0.0056(4) 0.0047(5) 0.0028(5) -0.0001(2) 0.0001(2)
    C11 0.0056(4) 0.0056(4) 0.0047(5) 0.0028(5) -0.0001(2) 0.0001(2)
    B2 0.0046(4) 0.0046(4) 0.0059(5) 0.0015(4) -0.0003(2) 0.0003(2)
    B3 0.0099(11) 0.0099(11) 0.016(2) 0.0049(6) 0 0
    C1 0.0041(6) 0.0041(6) 0.013(2) 0.0021(3) 0 0
    B11 0.0041(6) 0.0041(6) 0.013(2) 0.0021(3) 0 0
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes.
;
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
    B1 C11 19_665 1.731(3) ?
    B1 B1 19_665 1.731(3) ?
    B1 B2 . 1.801(2) ?
    B1 B2 28 1.8091(15) ?
    B1 B2 26_455 1.8091(15) ?
    B1 B1 4_565 1.825(3) ?
    B1 C11 4_565 1.825(3) ?
    B1 C11 2_665 1.825(3) ?
    B1 B1 2_665 1.825(3) ?
    B2 C1 25 1.6239(19) ?
    B2 B11 25 1.77(2) ?
    B2 B2 26_455 1.7778(17) ?
    B2 B2 28 1.7778(17) ?
    B2 C11 28 1.8091(15) ?
    B2 B1 28 1.8091(15) ?
    B2 C11 26_455 1.8091(15) ?
    B2 B1 26_455 1.8091(15) ?
    B3 B11 . 0.96(5) ?
    B3 B11 19 0.96(5) ?
    B3 C1 19 1.430(6) ?
    B3 C1 . 1.430(6) ?
    C1 B2 25 1.6239(19) ?
    C1 B2 26_455 1.6239(19) ?
    C1 B2 28_445 1.6239(19) ?
    B11 B2 25 1.77(2) ?
    B11 B2 26_455 1.77(2) ?
    B11 B2 28_445 1.77(2) ?
    B11 B11 19 1.92(9) ?
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_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    C11 B1 B1 19_665 19_665 0.00(8) ?
    C11 B1 B2 19_665 . 118.22(14) ?
    B1 B1 B2 19_665 . 118.22(14) ?
    C11 B1 B2 19_665 28 121.45(8) ?
    B1 B1 B2 19_665 28 121.45(8) ?
    B2 B1 B2 . 28 59.01(5) ?
    C11 B1 B2 19_665 26_455 121.45(8) ?
    B1 B1 B2 19_665 26_455 121.45(8) ?
    B2 B1 B2 . 26_455 59.01(5) ?
    B2 B1 B2 28 26_455 105.68(11) ?
    C11 B1 B1 19_665 4_565 125.36(8) ?
    B1 B1 B1 19_665 4_565 125.36(8) ?
    B2 B1 B1 . 4_565 107.10(6) ?
    B2 B1 B1 28 4_565 107.02(6) ?
    B2 B1 B1 26_455 4_565 59.72(5) ?
    C11 B1 C11 19_665 4_565 125.36(8) ?
    B1 B1 C11 19_665 4_565 125.36(8) ?
    B2 B1 C11 . 4_565 107.10(6) ?
    B2 B1 C11 28 4_565 107.02(6) ?
    B2 B1 C11 26_455 4_565 59.72(5) ?
    B1 B1 C11 4_565 4_565 0.00(9) ?
    C11 B1 C11 19_665 2_665 125.36(8) ?
    B1 B1 C11 19_665 2_665 125.36(8) ?
    B2 B1 C11 . 2_665 107.10(6) ?
    B2 B1 C11 28 2_665 59.72(5) ?
    B2 B1 C11 26_455 2_665 107.02(6) ?
    B1 B1 C11 4_565 2_665 60 ?
    C11 B1 C11 4_565 2_665 60 ?
    C11 B1 B1 19_665 2_665 125.36(8) ?
    B1 B1 B1 19_665 2_665 125.36(8) ?
    B2 B1 B1 . 2_665 107.10(6) ?
    B2 B1 B1 28 2_665 59.72(5) ?
    B2 B1 B1 26_455 2_665 107.02(6) ?
    B1 B1 B1 4_565 2_665 60 ?
    C11 B1 B1 4_565 2_665 60 ?
    C11 B1 B1 2_665 2_665 0.00(10) ?
    C1 B2 B11 25 25 15.1(12) ?
    C1 B2 B2 25 26_455 121.49(7) ?
    B11 B2 B2 25 26_455 125.0(2) ?
    C1 B2 B2 25 28 121.49(7) ?
    B11 B2 B2 25 28 125.0(2) ?
    B2 B2 B2 26_455 28 108.39(8) ?
    C1 B2 B1 25 . 119.9(2) ?
    B11 B2 B1 25 . 135.0(14) ?
    B2 B2 B1 26_455 . 60.73(7) ?
    B2 B2 B1 28 . 60.73(7) ?
    C1 B2 C11 25 28 121.07(19) ?
    B11 B2 C11 25 28 108.5(11) ?
    B2 B2 C11 26_455 28 108.78(7) ?
    B2 B2 C11 28 28 60.26(7) ?
    B1 B2 C11 . 28 110.05(9) ?
    C1 B2 B1 25 28 121.07(19) ?
    B11 B2 B1 25 28 108.5(11) ?
    B2 B2 B1 26_455 28 108.78(7) ?
    B2 B2 B1 28 28 60.26(7) ?
    B1 B2 B1 . 28 110.05(9) ?
    C11 B2 B1 28 28 0.00(11) ?
    C1 B2 C11 25 26_455 121.07(19) ?
    B11 B2 C11 25 26_455 108.5(11) ?
    B2 B2 C11 26_455 26_455 60.26(7) ?
    B2 B2 C11 28 26_455 108.78(7) ?
    B1 B2 C11 . 26_455 110.05(9) ?
    C11 B2 C11 28 26_455 60.56(11) ?
    B1 B2 C11 28 26_455 60.56(11) ?
    C1 B2 B1 25 26_455 121.07(19) ?
    B11 B2 B1 25 26_455 108.5(11) ?
    B2 B2 B1 26_455 26_455 60.26(7) ?
    B2 B2 B1 28 26_455 108.78(7) ?
    B1 B2 B1 . 26_455 110.05(9) ?
    C11 B2 B1 28 26_455 60.56(11) ?
    B1 B2 B1 28 26_455 60.56(11) ?
    C11 B2 B1 26_455 26_455 0.00(4) ?
    B11 B3 B11 . 19 180.0000(10) ?
    B11 B3 C1 . 19 180.0000(10) ?
    B11 B3 C1 19 19 0.0000(10) ?
    B11 B3 C1 . . 0.0000(10) ?
    B11 B3 C1 19 . 180.0000(10) ?
    C1 B3 C1 19 . 180 ?
    B3 C1 B2 . 25 100.1(2) ?
    B3 C1 B2 . 26_455 100.1(2) ?
    B2 C1 B2 25 26_455 117.01(13) ?
    B3 C1 B2 . 28_445 100.1(2) ?
    B2 C1 B2 25 28_445 117.01(13) ?
    B2 C1 B2 26_455 28_445 117.01(13) ?
    B3 B11 B2 . 25 115.2(13) ?
    B3 B11 B2 . 26_455 115.2(13) ?
    B2 B11 B2 25 26_455 103.2(16) ?
    B3 B11 B2 . 28_445 115.2(13) ?
    B2 B11 B2 25 28_445 103.2(16) ?
    B2 B11 B2 26_455 28_445 103.2(16) ?
    B3 B11 B11 . 19 0.0000(10) ?
    B2 B11 B11 25 19 115.2(13) ?
    B2 B11 B11 26_455 19 115.2(13) ?
    B2 B11 B11 28_445 19 115.2(13) ?
