#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/07/2010761.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_2010761
loop_
_publ_author_name
'Su, Cheng-Yong'
'Yang, Xiao-Ping'
'Xu, An-Wu'
'Zhang, Ze-Fu'
'Liu, Hong-Ke'
'Kang, Bei-Sheng'
_publ_section_title
;
 Hexakis(antipyrine-O)terbium(III) triperchlorate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e82
_journal_page_last               e83
_journal_paper_doi               10.1107/S0108270100002298
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C66 H72 N12 O6 Tb, 3(Cl O4)'
_chemical_formula_sum            'C66 H72 Cl3 N12 O18 Tb'
_chemical_formula_weight         1586.63
_chemical_name_systematic
;
Hexakis(antipyrine-O)terbium(III) triperchlorate
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   13.9691(10)
_cell_length_b                   13.9691(10)
_cell_length_c                   32.390(3)
_cell_measurement_reflns_used    980
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.8
_cell_measurement_theta_min      2.6
_cell_volume                     5473.7(8)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .998
_diffrn_measured_fraction_theta_max .998
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  .054
_diffrn_reflns_av_sigmaI/netI    .0439
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            12276
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.154
_exptl_absorpt_correction_T_max  .933
_exptl_absorpt_correction_T_min  .793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Multi-scan (Blessing, 1995)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2436
_exptl_crystal_size_max          .21
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .06
_refine_diff_density_max         .795
_refine_diff_density_min         -.498
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          .046
_refine_ls_R_factor_gt           .045
_refine_ls_shift/su_max          .017
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0697P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .110
_reflns_number_gt                2688
_reflns_number_total             2800
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            qb0180.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5473.6(8)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2010761
_cod_database_fobs_code          2010761
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'
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
Tb1 .0000 .0000 .0000 .03472(15) Uani d S 1 . . Tb
O1 -.11759(18) .02504(19) .04133(7) .0434(5) Uani d . 1 . . O
N1 -.2737(2) .0377(2) .05057(9) .0451(6) Uani d . 1 . . N
N2 -.3318(3) .0436(3) .08415(11) .0645(9) Uani d . 1 . . N
C1 -.1882(3) .0242(3) .06515(10) .0394(7) Uani d . 1 . . C
C2 -.1998(3) .0159(3) .10838(11) .0581(9) Uani d . 1 . . C
H2 -.1551 .0050 .1268 .070 Uiso calc R 1 . . H
C3 -.2884(4) .0268(4) .11809(13) .0698(12) Uani d . 1 . . C
C4 -.3377(6) .0192(6) .16031(17) .122(3) Uani d . 1 . . C
H4A -.3900 .0446 .1588 .182 Uiso calc PR .50 . . H
H4B -.2800 .0644 .1794 .182 Uiso calc PR .50 . . H
H4C -.3744 -.0562 .1695 .182 Uiso calc PR .50 . . H
H4D -.3062 -.0094 .1797 .182 Uiso calc PR .50 . . H
H4E -.4163 -.0292 .1591 .182 Uiso calc PR .50 . . H
H4F -.3219 .0914 .1690 .182 Uiso calc PR .50 . . H
C5 -.4457(4) .0215(5) .07828(19) .0903(17) Uani d . 1 . . C
H5A -.4628 .0141 .0493 .136 Uiso calc PR .50 . . H
H5B -.4523 .0816 .0894 .136 Uiso calc PR .50 . . H
H5C -.4963 -.0458 .0922 .136 Uiso calc PR .50 . . H
H5D -.4781 .0192 .1047 .136 Uiso calc PR .50 . . H
H5E -.4886 -.0483 .0646 .136 Uiso calc PR .50 . . H
H5F -.4447 .0791 .0618 .136 Uiso calc PR .50 . . H
C6 -.2749(2) .0830(3) .01147(11) .0433(7) Uani d . 1 . . C
C7 -.2754(3) .0264(3) -.02312(11) .0507(8) Uani d . 1 . . C
H7 -.2816 -.0429 -.0207 .061 Uiso calc R 1 . . H
C8 -.2666(4) .0724(5) -.06146(15) .0815(15) Uani d . 1 . . C
H8 -.2654 .0340 -.0847 .098 Uiso calc R 1 . . H
C9 -.2599(4) .1685(7) -.0661(2) .104(2) Uani d . 1 . . C
H9 -.2549 .1971 -.0925 .124 Uiso calc R 1 . . H
C10 -.2602(4) .2273(5) -.0322(3) .103(2) Uani d . 1 . . C
H10 -.2556 .2956 -.0357 .123 Uiso calc R 1 . . H
C11 -.2673(3) .1857(4) .00741(19) .0725(13) Uani d . 1 . . C
H11 -.2670 .2254 .0305 .087 Uiso calc R 1 . . H
Cl1 .6667 .3333 .11996(6) .0738(5) Uani d S 1 . . Cl
O12 .6667 .3333 .0778(3) .131(3) Uani d S 1 . . O
O11 .5646(6) .2555(7) .1302(3) .241(4) Uani d . 1 . . O
Cl2 -.3333 .3333 -.1667 .0779(8) Uani d S 1 . . Cl
O22 -.3333 .3333 -.1264(6) .152(8) Uani d SP .50 . . O
O21 -.2661(15) .4378(11) -.1819(4) .187(5) Uani d P .50 . . O
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'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 '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'
Tb Tb -.1723 4.1537 '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_site_symmetry_3
_geom_angle
O1 Tb1 O1 12 3 180
O1 Tb1 O1 12 11 88.96(8)
O1 Tb1 O1 3 11 91.04(8)
O1 Tb1 O1 12 . 91.04(8)
O1 Tb1 O1 3 . 88.96(8)
O1 Tb1 O1 11 . 91.04(8)
O1 Tb1 O1 12 2 91.04(8)
O1 Tb1 O1 3 2 88.96(8)
O1 Tb1 O1 11 2 180
O1 Tb1 O1 . 2 88.96(8)
O1 Tb1 O1 12 10 88.96(8)
O1 Tb1 O1 3 10 91.04(8)
O1 Tb1 O1 11 10 88.96(8)
O1 Tb1 O1 . 10 180
O1 Tb1 O1 2 10 91.04(8)
C1 O1 Tb1 . . 171.7(2)
C1 N1 N2 . . 108.2(3)
C1 N1 C6 . . 124.7(3)
N2 N1 C6 . . 122.5(3)
C3 N2 N1 . . 107.8(3)
C3 N2 C5 . . 127.5(4)
N1 N2 C5 . . 119.3(4)
O1 C1 N1 . . 121.4(3)
O1 C1 C2 . . 132.3(3)
N1 C1 C2 . . 106.2(3)
C3 C2 C1 . . 107.2(4)
C3 C2 H2 . . 126.4
C1 C2 H2 . . 126.4
N2 C3 C2 . . 110.5(3)
N2 C3 C4 . . 121.9(5)
C2 C3 C4 . . 127.7(5)
C3 C4 H4A . . 109.5
C3 C4 H4B . . 109.5
H4A C4 H4B . . 109.5
C3 C4 H4C . . 109.5
H4A C4 H4C . . 109.5
H4B C4 H4C . . 109.5
C3 C4 H4D . . 109.5
H4A C4 H4D . . 141.1
H4B C4 H4D . . 56.3
H4C C4 H4D . . 56.3
C3 C4 H4E . . 109.5
H4A C4 H4E . . 56.3
H4B C4 H4E . . 141.1
H4C C4 H4E . . 56.3
H4D C4 H4E . . 109.5
C3 C4 H4F . . 109.5
H4A C4 H4F . . 56.3
H4B C4 H4F . . 56.3
H4C C4 H4F . . 141.1
H4D C4 H4F . . 109.5
H4E C4 H4F . . 109.5
N2 C5 H5A . . 109.5
N2 C5 H5B . . 109.5
H5A C5 H5B . . 109.5
N2 C5 H5C . . 109.5
H5A C5 H5C . . 109.5
H5B C5 H5C . . 109.5
N2 C5 H5D . . 109.5
H5A C5 H5D . . 141.1
H5B C5 H5D . . 56.3
H5C C5 H5D . . 56.3
N2 C5 H5E . . 109.5
H5A C5 H5E . . 56.3
H5B C5 H5E . . 141.1
H5C C5 H5E . . 56.3
H5D C5 H5E . . 109.5
N2 C5 H5F . . 109.5
H5A C5 H5F . . 56.3
H5B C5 H5F . . 56.3
H5C C5 H5F . . 141.1
H5D C5 H5F . . 109.5
H5E C5 H5F . . 109.5
C7 C6 C11 . . 119.6(4)
C7 C6 N1 . . 118.0(3)
C11 C6 N1 . . 122.1(4)
C6 C7 C8 . . 119.7(4)
C6 C7 H7 . . 120.2
C8 C7 H7 . . 120.2
C9 C8 C7 . . 121.9(6)
C9 C8 H8 . . 119.1
C7 C8 H8 . . 119.1
C8 C9 C10 . . 120.2(6)
C8 C9 H9 . . 119.9
C10 C9 H9 . . 119.9
C9 C10 C11 . . 120.5(5)
C9 C10 H10 . . 119.7
C11 C10 H10 . . 119.7
C6 C11 C10 . . 118.1(5)
C6 C11 H11 . . 121.0
C10 C11 H11 . . 121.0
O11 Cl1 O11 2_655 . 114.0(3)
O11 Cl1 O11 2_655 3_665 114.0(3)
O11 Cl1 O11 . 3_665 114.0(3)
O11 Cl1 O12 2_655 . 104.5(4)
O11 Cl1 O12 . . 104.5(4)
O11 Cl1 O12 3_665 . 104.5(4)
O22 Cl2 O22 . 16_454 180
O22 Cl2 O21 . 18_554 68.9(6)
O22 Cl2 O21 16_454 18_554 111.1(6)
O22 Cl2 O21 . 3_455 111.1(6)
O22 Cl2 O21 16_454 3_455 68.9(6)
O21 Cl2 O21 18_554 3_455 179.998(4)
O22 Cl2 O21 . 16_454 68.9(6)
O22 Cl2 O21 16_454 16_454 111.1(6)
O21 Cl2 O21 18_554 16_454 107.8(7)
O21 Cl2 O21 3_455 16_454 72.2(7)
O22 Cl2 O21 . . 111.1(6)
O22 Cl2 O21 16_454 . 68.9(6)
O21 Cl2 O21 18_554 . 72.2(7)
O21 Cl2 O21 3_455 . 107.8(7)
O21 Cl2 O21 16_454 . 180
O22 Cl2 O21 . 2_565 111.1(6)
O22 Cl2 O21 16_454 2_565 68.9(6)
O21 Cl2 O21 18_554 2_565 72.2(7)
O21 Cl2 O21 3_455 2_565 107.8(7)
O21 Cl2 O21 16_454 2_565 72.2(7)
O21 Cl2 O21 . 2_565 107.8(7)
O22 Cl2 O21 . 17_444 68.9(6)
O22 Cl2 O21 16_454 17_444 111.1(6)
O21 Cl2 O21 18_554 17_444 107.8(7)
O21 Cl2 O21 3_455 17_444 72.2(7)
O21 Cl2 O21 16_454 17_444 107.8(7)
O21 Cl2 O21 . 17_444 72.2(7)
O21 Cl2 O21 2_565 17_444 180
Cl2 O22 O21 . 18_554 57.7(8)
Cl2 O22 O21 . 16_454 57.7(8)
O21 O22 O21 18_554 16_454 94.1(10)
Cl2 O22 O21 . 17_444 57.7(8)
O21 O22 O21 18_554 17_444 94.1(10)
O21 O22 O21 16_454 17_444 94.1(10)
Cl2 O21 O22 . 16_454 53.4(8)
Cl2 O21 O21 . 18_554 53.9(3)
O22 O21 O21 16_454 18_554 89.5(7)
Cl2 O21 O21 . 17_444 53.9(3)
O22 O21 O21 16_454 17_444 89.5(7)
O21 O21 O21 18_554 17_444 86.6(13)
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
Tb1 O1 12 2.278(2) ?
Tb1 O1 3 2.278(2) ?
Tb1 O1 11 2.278(2) ?
Tb1 O1 . 2.278(2) ?
Tb1 O1 2 2.278(2) ?
Tb1 O1 10 2.278(2) ?
O1 C1 . 1.248(4) ?
N1 C1 . 1.382(4) ?
N1 N2 . 1.384(4) ?
N1 C6 . 1.420(5) ?
N2 C3 . 1.332(6) ?
N2 C5 . 1.474(5) ?
C1 C2 . 1.408(5) ?
C2 C3 . 1.357(6) ?
C2 H2 . .9300 ?
C3 C4 . 1.511(6) ?
C4 H4A . .9600 ?
C4 H4B . .9600 ?
C4 H4C . .9600 ?
C4 H4D . .9600 ?
C4 H4E . .9600 ?
C4 H4F . .9600 ?
C5 H5A . .9600 ?
C5 H5B . .9600 ?
C5 H5C . .9600 ?
C5 H5D . .9600 ?
C5 H5E . .9600 ?
C5 H5F . .9600 ?
C6 C7 . 1.370(5) ?
C6 C11 . 1.391(5) ?
C7 C8 . 1.375(6) ?
C7 H7 . .9300 ?
C8 C9 . 1.307(9) ?
C8 H8 . .9300 ?
C9 C10 . 1.373(9) ?
C9 H9 . .9300 ?
C10 C11 . 1.392(9) ?
C10 H10 . .9300 ?
C11 H11 . .9300 ?
Cl1 O11 2_655 1.333(6) ?
Cl1 O11 . 1.333(6) ?
Cl1 O11 3_665 1.333(6) ?
Cl1 O12 . 1.365(8) ?
Cl2 O22 . 1.303(18) ?
Cl2 O22 16_454 1.303(18) ?
Cl2 O21 18_554 1.373(11) ?
Cl2 O21 3_455 1.373(11) ?
Cl2 O21 16_454 1.373(11) ?
Cl2 O21 . 1.373(11) ?
Cl2 O21 2_565 1.373(11) ?
Cl2 O21 17_444 1.373(11) ?
O22 O21 18_554 1.516(16) ?
O22 O21 16_454 1.516(17) ?
O22 O21 17_444 1.516(16) ?
O21 O22 16_454 1.516(16) ?
O21 O21 18_554 1.618(17) ?
O21 O21 17_444 1.618(17) ?
