##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
##############################################################################
#                                                                            #
# 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 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. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
#                                                                            #
##############################################################################
                                             
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common     ?
_chemical_formula_moiety     'C66 H72 N12 O6 Tb1 3+, 3 I 1-'
_chemical_formula_sum     'C66 H72 I3 N12 O6 Tb'
_chemical_formula_iupac     '[Tb (C11 H12 N2 O)6] I3'
_chemical_formula_weight     1668.98
_chemical_melting_point     ?
_symmetry_cell_setting     rhombohedral
_symmetry_space_group_name_H-M     'R -3'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-y, x-y, z'
    '-x+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+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, -z'
    'y, -x+y, -z'
    'x-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+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'
_cell_length_a     13.7474(3)
_cell_length_b     13.7474(3)
_cell_length_c     31.9658(14)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     120.00
_cell_volume     5231.9(3)
_cell_formula_units_Z     3
_cell_measurement_reflns_used     12573
_cell_measurement_theta_min     3.0
_cell_measurement_theta_max     28.9
_cell_measurement_temperature     160(2)
_exptl_crystal_description     block
_exptl_crystal_colour     colourless
_exptl_crystal_size_max     0.50
_exptl_crystal_size_mid     0.40
_exptl_crystal_size_min     0.35
_exptl_crystal_density_diffrn     1.589
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     2472
_exptl_absorpt_coefficient_mu     2.398
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(SADABS; Sheldrick, 1997a)'
_exptl_absorpt_correction_T_min     0.387
_exptl_absorpt_correction_T_max     0.492
_exptl_special_details
;
 ?
;
_diffrn_ambient_temperature     160(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Bruker SMART 1K CCD'
_diffrn_measurement_method     'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean     8.192
_diffrn_reflns_number     15672
_diffrn_reflns_av_R_equivalents     0.0195
_diffrn_reflns_av_sigmaI/netI     0.0140
_diffrn_reflns_theta_min     1.8
_diffrn_reflns_theta_max     28.9
_diffrn_reflns_theta_full     26.0
_diffrn_measured_fraction_theta_max     0.963
_diffrn_measured_fraction_theta_full     1.000
_diffrn_reflns_limit_h_min     -17
_diffrn_reflns_limit_h_max     17
_diffrn_reflns_limit_k_min     -18
_diffrn_reflns_limit_k_max     18
_diffrn_reflns_limit_l_min     -43
_diffrn_reflns_limit_l_max     43
_diffrn_standards_number     0
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     0
_refine_special_details
;
 ?
;
_reflns_number_total     2945
_reflns_number_gt     2692
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0224
_refine_ls_R_factor_gt     0.0185
_refine_ls_wR_factor_gt     0.0459
_refine_ls_wR_factor_ref     0.0474
_refine_ls_goodness_of_fit_ref     1.098
_refine_ls_restrained_S_all     1.098
_refine_ls_number_reflns     2945
_refine_ls_number_parameters     137
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
          'w = 1/[σ²(Fo²)+(0.0204P)²+8.1659P] where P = (Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     <0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.347
_refine_diff_density_min     -0.766
_refine_ls_extinction_method     SHELXTL
_refine_ls_extinction_coef     0.00009(3)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
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'
    'N' 'N' 0.0061 0.0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O' 0.0106 0.0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'I' 'I' -0.4742 1.8119
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Tb' 'Tb' -0.1723 4.1537
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'SMART (Bruker, 1997)'
_computing_cell_refinement     'SAINT (Bruker, 1997)'
_computing_data_reduction     'SAINT'
_computing_structure_solution     'SHELXTL (Sheldrick, 1997b)'
_computing_structure_refinement     SHELXTL
_computing_molecular_graphics     SHELXTL
_computing_publication_material     'SHELXTL and local programs'
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_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Tb 0.0000 0.0000 0.0000 0.01863(6) Uani d S 1 . . Tb
    O1 -0.11349(10) 0.02865(10) 0.04196(4) 0.0281(3) Uani d . 1 . . O
    N1 -0.33249(14) 0.04546(16) 0.08622(5) 0.0415(4) Uani d . 1 . . N
    N2 -0.27309(12) 0.04007(13) 0.05215(5) 0.0298(3) Uani d . 1 . . N
    C1 -0.18594(14) 0.02658(14) 0.06669(5) 0.0253(3) Uani d . 1 . . C
    C2 -0.19706(17) 0.01697(17) 0.11044(6) 0.0363(4) Uani d . 1 . . C
    H2 -0.1500 0.0058 0.1293 0.044 Uiso calc R 1 . . H
    C3 -0.28844(19) 0.0268(2) 0.12084(6) 0.0447(5) Uani d . 1 . . C
    C4 -0.3408(3) 0.0167(3) 0.16288(8) 0.0754(9) Uani d . 1 . . C
    H4A -0.3537 0.0800 0.1671 0.113 Uiso calc R 1 . . H
    H4B -0.2903 0.0176 0.1847 0.113 Uiso calc R 1 . . H
    H4C -0.4125 -0.0539 0.1644 0.113 Uiso calc R 1 . . H
    C5 -0.44747(18) 0.0240(2) 0.08044(9) 0.0561(6) Uani d . 1 . . C
    H5A -0.5010 -0.0523 0.0898 0.084 Uiso calc R 1 . . H
    H5B -0.4602 0.0320 0.0508 0.084 Uiso calc R 1 . . H
    H5C -0.4580 0.0782 0.0969 0.084 Uiso calc R 1 . . H
    C6 -0.27165(14) 0.09003(15) 0.01298(6) 0.0286(3) Uani d . 1 . . C
    C7 -0.26096(18) 0.19576(18) 0.01085(9) 0.0513(6) Uani d . 1 . . C
    H7 -0.2608 0.2346 0.0354 0.062 Uiso calc R 1 . . H
    C8 -0.2505(2) 0.2430(2) -0.02876(13) 0.0748(10) Uani d . 1 . . C
    H8 -0.2436 0.3151 -0.0310 0.090 Uiso calc R 1 . . H
    C9 -0.2498(2) 0.1883(3) -0.06428(11) 0.0733(10) Uani d . 1 . . C
    H9 -0.2429 0.2220 -0.0909 0.088 Uiso calc R 1 . . H
    C10 -0.25923(18) 0.0851(2) -0.06136(7) 0.0544(6) Uani d . 1 . . C
    H10 -0.2576 0.0474 -0.0860 0.065 Uiso calc R 1 . . H
    C11 -0.27111(15) 0.03450(17) -0.02277(6) 0.0337(4) Uani d . 1 . . C
    H11 -0.2788 -0.0380 -0.0210 0.040 Uiso calc R 1 . . H
    I1 -0.3333 0.3333 0.124103(7) 0.04370(8) Uani d S 1 . . I
    I2 -0.3333 0.3333 -0.1667 0.05569(11) Uani d S 1 . . I
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
    Tb 0.01812(7) 0.01812(7) 0.01965(9) 0.00906(3) 0.000 0.000
    O1 0.0272(6) 0.0347(6) 0.0280(6) 0.0197(5) 0.0042(5) 0.0027(5)
    N1 0.0325(8) 0.0607(11) 0.0376(9) 0.0280(8) 0.0087(7) -0.0089(8)
    N2 0.0265(7) 0.0415(8) 0.0271(7) 0.0214(7) 0.0020(6) -0.0050(6)
    C1 0.0235(8) 0.0262(8) 0.0260(8) 0.0123(6) 0.0005(6) -0.0011(6)
    C2 0.0382(10) 0.0435(11) 0.0251(9) 0.0187(9) 0.0009(7) -0.0009(8)
    C3 0.0459(12) 0.0555(13) 0.0308(10) 0.0239(10) 0.0105(9) -0.0046(9)
    C4 0.084(2) 0.110(3) 0.0389(13) 0.053(2) 0.0273(13) 0.0004(14)
    C5 0.0311(11) 0.0680(16) 0.0738(17) 0.0282(11) 0.0072(10) -0.0171(13)
    C6 0.0212(7) 0.0289(8) 0.0379(9) 0.0142(7) -0.0026(7) -0.0009(7)
    C7 0.0363(11) 0.0365(11) 0.0894(18) 0.0243(9) -0.0062(11) -0.0031(11)
    C8 0.0402(13) 0.0511(15) 0.140(3) 0.0280(12) 0.0030(16) 0.0432(18)
    C9 0.0369(12) 0.097(2) 0.084(2) 0.0323(14) 0.0048(13) 0.0540(19)
    C10 0.0342(11) 0.0852(18) 0.0357(11) 0.0237(12) -0.0052(9) 0.0129(11)
    C11 0.0277(9) 0.0391(10) 0.0323(9) 0.0152(8) -0.0052(7) -0.0014(8)
    I1 0.04874(10) 0.04874(10) 0.03362(12) 0.02437(5) 0.000 0.000
    I2 0.06590(16) 0.06590(16) 0.03527(18) 0.03295(8) 0.000 0.000
_geom_special_details
;
 ?
;
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
    Tb O1 . 2.2367(11) yes
    Tb O1 12 2.2367(11) ?
    Tb O1 3 2.2367(11) ?
    Tb O1 11 2.2367(11) ?
    Tb O1 2 2.2367(11) ?
    Tb O1 10 2.2367(11) ?
    O1 C1 . 1.261(2) yes
    N1 N2 . 1.385(2) yes
    N1 C3 . 1.347(3) yes
    N1 C5 . 1.468(3) ?
    N2 C1 . 1.381(2) yes
    N2 C6 . 1.423(2) ?
    C1 C2 . 1.406(2) yes
    C2 H2 . 0.950 ?
    C2 C3 . 1.370(3) yes
    C3 C4 . 1.498(3) ?
    C4 H4A . 0.980 ?
    C4 H4B . 0.980 ?
    C4 H4C . 0.980 ?
    C5 H5A . 0.980 ?
    C5 H5B . 0.980 ?
    C5 H5C . 0.980 ?
    C6 C7 . 1.388(3) ?
    C6 C11 . 1.376(3) ?
    C7 H7 . 0.950 ?
    C7 C8 . 1.397(4) ?
    C8 H8 . 0.950 ?
    C8 C9 . 1.364(5) ?
    C9 H9 . 0.950 ?
    C9 C10 . 1.363(4) ?
    C10 H10 . 0.950 ?
    C10 C11 . 1.385(3) ?
    C11 H11 . 0.950 ?
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
    O1 Tb O1 12 3 180.0 ?
    O1 Tb O1 12 11 87.75(4) ?
    O1 Tb O1 3 11 92.25(4) ?
    O1 Tb O1 . 12 92.25(4) ?
    O1 Tb O1 . 3 87.75(4) yes
    O1 Tb O1 . 11 92.25(4) yes
    O1 Tb O1 12 2 92.25(4) ?
    O1 Tb O1 3 2 87.75(4) ?
    O1 Tb O1 11 2 180.0 ?
    O1 Tb O1 . 2 87.75(4) ?
    O1 Tb O1 12 10 87.75(4) ?
    O1 Tb O1 3 10 92.25(4) ?
    O1 Tb O1 11 10 87.75(4) ?
    O1 Tb O1 . 10 180.0 yes
    O1 Tb O1 2 10 92.25(4) ?
    Tb O1 C1 . . 170.00(12) yes
    N2 N1 C3 . . 107.60(15) yes
    N2 N1 C5 . . 119.66(17) ?
    C3 N1 C5 . . 127.39(19) ?
    N1 N2 C1 . . 108.47(14) yes
    N1 N2 C6 . . 122.15(15) ?
    C1 N2 C6 . . 123.85(14) ?
    O1 C1 N2 . . 120.96(15) yes
    O1 C1 C2 . . 132.34(17) yes
    N2 C1 C2 . . 106.65(15) yes
    C1 C2 H2 . . 126.4 ?
    C1 C2 C3 . . 107.11(18) yes
    H2 C2 C3 . . 126.4 ?
    N1 C3 C2 . . 109.97(17) yes
    N1 C3 C4 . . 120.9(2) ?
    C2 C3 C4 . . 129.1(2) ?
    C3 C4 H4A . . 109.5 ?
    C3 C4 H4B . . 109.5 ?
    C3 C4 H4C . . 109.5 ?
    H4A C4 H4B . . 109.5 ?
    H4A C4 H4C . . 109.5 ?
    H4B C4 H4C . . 109.5 ?
    N1 C5 H5A . . 109.5 ?
    N1 C5 H5B . . 109.5 ?
    N1 C5 H5C . . 109.5 ?
    H5A C5 H5B . . 109.5 ?
    H5A C5 H5C . . 109.5 ?
    H5B C5 H5C . . 109.5 ?
    N2 C6 C7 . . 121.15(19) ?
    N2 C6 C11 . . 117.73(16) ?
    C7 C6 C11 . . 120.9(2) ?
    C6 C7 H7 . . 121.2 ?
    C6 C7 C8 . . 117.6(3) ?
    H7 C7 C8 . . 121.2 ?
    C7 C8 H8 . . 119.1 ?
    C7 C8 C9 . . 121.8(2) ?
    H8 C8 C9 . . 119.1 ?
    C8 C9 H9 . . 120.2 ?
    C8 C9 C10 . . 119.6(2) ?
    H9 C9 C10 . . 120.2 ?
    C9 C10 H10 . . 119.7 ?
    C9 C10 C11 . . 120.6(3) ?
    H10 C10 C11 . . 119.7 ?
    C6 C11 C10 . . 119.5(2) ?
    C6 C11 H11 . . 120.2 ?
    C10 C11 H11 . . 120.2 ?
data_global
_journal_date_recd_electronic     2002-03-15
_journal_date_accepted     2002-03-19
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2002
_journal_volume     58
_journal_issue      4
_journal_page_first     m159
_journal_page_last     m161
_journal_paper_category     EM
_publ_contact_author_name     'Professor W. Clegg'
_publ_contact_author_address
;
Department of Chemistry
Bedson Building
University of Newcastle
Newcastle upon Tyne NE1 7RU
;
_publ_contact_author_email     w.clegg@ncl.ac.uk
_publ_contact_author_fax     '0191 222 6929'
_publ_contact_author_phone     '0191 222 6649'
_publ_section_title
; Hexakis(antipyrine-O)terbium(III) triiodide at 160 K: confirmation of
a centrosymmetric structure for a brilliantly triboluminescent complex
;
_publ_section_title_footnote
;
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Clegg, William' .
; Department of Chemistry
  University of Newcastle upon Tyne
  Newcastle upon Tyne NE1 7RU
  England
;
    'Bourhill, Grant'
; Present address: Sharp Labs of Europe
 Edmund Halley Road
 Oxford Science Park
 Oxford OX4 4GB
 England
;
; Sensors & Electronics Division
  E-1201
  QinetiQ
  Malvern WR14 3PS
  England
;
    'Sage, Ian' .
; Sensors & Electronics Division
  E-1201
  QinetiQ
  Malvern WR14 3PS
  England
;
