#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/54/2005427.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_2005427
loop_
_publ_author_name
'Smyth, M. V.'
'Bailey, R. D.'
'Pennington, W. T.'
_publ_section_title
;
 Tetrakis(2,3,5,6-tetramethylpyrazinium)
 Tetra-μ₃-iodo-hexa-μ-iodo-dodecaiodohexaantimonate(4--)
 Tetrahydrate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2170
_journal_page_last               2173
_journal_paper_doi               10.1107/S0108270196006038
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '(C8 H13 N2)4 , [Sb6 I22] , 4H2 O'
_chemical_formula_sum            'C32 H60 I22 N8 O4 Sb6'
_chemical_formula_weight         4143.18
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source           'Cromer & Waber (1974)'
_cell_angle_alpha                89.588(2)
_cell_angle_beta                 84.336(2)
_cell_angle_gamma                68.014(2)
_cell_formula_units_Z            1
_cell_length_a                   11.4291(8)
_cell_length_b                   13.6877(9)
_cell_length_c                   15.488(1)
_cell_measurement_reflns_used    148
_cell_measurement_temperature    294(1)
_cell_measurement_theta_max      13.3
_cell_measurement_theta_min      6.5
_cell_volume                     2234.6(3)
_diffrn_measurement_device       'Syntex P2₁'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6336
_diffrn_reflns_theta_max         22.5
_diffrn_standards_decay_%        .0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.42
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.34
_exptl_absorpt_correction_type   'empirical, \y scans (SHELXTL-Plus)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.08
_exptl_crystal_description       parallelpiped
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.88
_refine_diff_density_min         -2.12
_refine_ls_extinction_coef       1.88E-6(8)
_refine_ls_extinction_method     'isotropic (Larson, 1970)'
_refine_ls_goodness_of_fit_obs   2.54
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4524
_refine_ls_R_factor_obs          0.0633
_refine_ls_shift/esd_max         0.005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F)+0.0005(F²)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0809
_reflns_number_observed          4524
_reflns_number_total             5863
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            sz1036.cif
_cod_data_source_block           ttt
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/[\s^2^(F)+0.0005(F^2^)]' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(F)+0.0005(F^2^)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2234.6(2)
_cod_database_code               2005427
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
I(1) .4380(1) .4493(1) .3847(1) .049(1)
I(2) .7015(1) .6139(1) .3621(1) .060(1)
I(3) .3168(1) .7781(1) .3059(1) .061(1)
I(4) .4468(2) .8632(1) .5288(1) .081(1)
I(5) .8172(1) .2915(1) .4468(1) .065(1)
I(6) .5750(1) .5143(1) .1318(1) .060(1)
I(7) .6989(2) .2028(1) .1985(1) .081(1)
I(8) .9534(1) .3560(1) .1809(1) .079(1)
I(9) .8303(1) .6827(1) .0929(1) .070(1)
I(10) .4504(1) .8190(1) .0433(1) .072(1)
I(11) .5917(2) .9422(1) .2410(1) .097(1)
Sb(1) .4377(1) .6780(1) .4606(1) .048(1)
Sb(2) .7114(1) .3881(1) .2628(1) .052(1)
Sb(3) .5891(1) .7488(1) .1852(1) .056(1)
O(1) .3373(14) .2469(10) .2910(10) .096(7)
O(2) -.0480(14) .8791(10) .1807(10) .087(7)
N(1) .2230(13) .1127(9) .2588(8) .047(5)
N(2) .0620(13) .0242(10) .2223(10) .055(6)
N(3) .0827(14) .6728(11) .2200(9) .056(7)
N(4) .1881(15) .4657(11) .2484(9) .060(7)
C(1) .2131(17) .0984(12) .1766(12) .058(8)
C(2) .1590(18) .0836(13) .3258(12) .062(8)
C(3) .0726(17) .0380(12) .3026(12) .060(8)
C(4) .1243(17) .0533(14) .1586(12) .062(8)
C(5) .2951(19) .1279(15) .1065(14) .074(9)
C(6) .182(2) .1018(16) .4163(11) .079(10)
C(7) -.008(2) .0011(16) .3722(13) .079(10)
C(8) .101(2) .0385(16) .0659(12) .081(10)
C(9) .0540(18) .6405(15) .2972(11) .063(9)
C(10) .1632(19) .6068(15) .1576(11) .064(9)
C(11) .2146(16) .5010(13) .1733(10) .051(7)
C(12) .1088(18) .5332(15) .3132(12) .064(9)
C(13) -.0379(18) .7251(13) .3616(11) .063(8)
C(14) .188(2) .6514(17) .0691(12) .080(10)
C(15) .300(2) .4198(15) .1058(12) .074(9)
C(16) .081(2) .4882(16) .3989(12) .076(10)
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
Sb(1) I(1) Sb(2) . . 94.50(10) yes
Sb(2) I(1) Sb(1) . 2_666 93.50(10) yes
Sb(1) I(2) Sb(3) . . 93.20(10) yes
Sb(1) I(3) Sb(3) . . 95.50(10) yes
Sb(2) I(6) Sb(3) . . 99.90(10) yes
I(1) Sb(1) I(3) . . 88.00(10) yes
I(1) Sb(1) I(4) . . 177.20(10) yes
I(3) Sb(1) I(4) . . 94.60(10) yes
I(2) Sb(1) I(1) . 2_666 88.60(10) yes
I(4) Sb(1) I(1) . 2_666 91.70(10) yes
I(2) Sb(1) I(5) . 2_666 171.70(10) yes
I(4) Sb(1) I(5) . 2_666 95.10(10) yes
I(1) Sb(2) I(2) . . 81.10(10) yes
I(2) Sb(2) I(5) . . 80.70(10) yes
I(2) Sb(2) I(6) . . 88.40(10) yes
I(1) Sb(2) I(7) . . 92.50(10) yes
I(5) Sb(2) I(7) . . 95.90(10) yes
I(1) Sb(2) I(8) . . 170.20(10) yes
I(5) Sb(2) I(8) . . 93.90(10) yes
I(7) Sb(2) I(8) . . 96.20(10) yes
I(2) Sb(3) I(6) . . 80.80(10) yes
I(2) Sb(3) I(9) . . 92.90(10) yes
I(6) Sb(3) I(9) . . 88.70(10) yes
I(3) Sb(3) I(10) . . 88.50(10) yes
I(9) Sb(3) I(10) . . 96.90(10) yes
I(3) Sb(3) I(11) . . 94.40(10) yes
I(9) Sb(3) I(11) . . 94.6(11) yes
C(1) N(1) C(2) . . 125(2) yes
C(9) N(3) C(10) . . 123(2) yes
N(1) C(1) C(4) . . 116(2) yes
C(4) C(1) C(5) . . 123(2) yes
N(1) C(2) C(6) . . 119(2) yes
N(2) C(3) C(2) . . 120(2) yes
C(2) C(3) C(7) . . 120(2) yes
N(2) C(4) C(8) . . 120(2) yes
N(3) C(9) C(12) . . 118(2) yes
C(12) C(9) C(13) . . 125(2) yes
N(3) C(10) C(14) . . 119(2) yes
N(4) C(11) C(10) . . 120.0(10) yes
C(10) C(11) C(15) . . 123(2) yes
N(4) C(12) C(16) . . 119(2) yes
Sb(1) I(1) Sb(1) . 2_666 94.30(10) yes
Sb(1) I(2) Sb(2) . . 98.00(10) yes
Sb(2) I(2) Sb(3) . . 89.40(10) yes
Sb(2) I(5) Sb(1) . 2_666 95.80(10) yes
I(1) Sb(1) I(2) . . 86.00(10) yes
I(2) Sb(1) I(3) . . 91.40(10) yes
I(2) Sb(1) I(4) . . 92.90(10) yes
I(1) Sb(1) I(1) . 2_666 85.70(10) yes
I(3) Sb(1) I(1) . 2_666 173.70(10) yes
I(1) Sb(1) I(5) . 2_666 85.90(10) yes
I(3) Sb(1) I(5) . 2_666 90.30(10) yes
I(1) Sb(1) I(5) 2_666 2_666 88.80(10) yes
I(1) Sb(2) I(5) . . 80.70(10) yes
I(1) Sb(2) I(6) . . 88.00(10) yes
I(5) Sb(2) I(6) . . 165.30(10) yes
I(2) Sb(2) I(7) . . 173.10(10) yes
I(6) Sb(2) I(7) . . 93.90(10) yes
I(2) Sb(2) I(8) . . 90.00(10) yes
I(6) Sb(2) I(8) . . 95.90(10) yes
I(2) Sb(3) I(3) . . 79.30(10) yes
I(3) Sb(3) I(6) . . 82.10(10) yes
I(3) Sb(3) I(9) . . 168.70(10) yes
I(2) Sb(3) I(10) . . 161.40(10) yes
I(6) Sb(3) I(10) . . 83.60(10) yes
I(2) Sb(3) I(11) . . 96.50(10) yes
I(6) Sb(3) I(11) . . 175.90(10) yes
I(10) Sb(3) I(11) . . 98.40(10) yes
C(3) N(2) C(4) . . 123(2) yes
C(11) N(4) C(12) . . 121(2) yes
N(1) C(1) C(5) . . 120(2) yes
N(1) C(2) C(3) . . 116(2) yes
C(3) C(2) C(6) . . 125(2) yes
N(2) C(3) C(7) . . 120(2) yes
N(2) C(4) C(1) . . 120(2) yes
C(1) C(4) C(8) . . 120(2) yes
N(3) C(9) C(13) . . 117(2) yes
N(3) C(10) C(11) . . 119(2) yes
C(11) C(10) C(14) . . 122(2) yes
N(4) C(11) C(15) . . 117(2) yes
N(4) C(12) C(9) . . 119(2) yes
C(9) C(12) C(16) . . 122(2) yes
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
I(1) Sb(1) . 3.351(2) yes
I(1) Sb(1) 2_666 3.0910(10) yes
I(2) Sb(2) . 3.421(2) yes
I(3) Sb(1) . 2.953(2) yes
I(4) Sb(1) . 2.794(2) yes
I(5) Sb(1) 2_666 2.999(2) yes
I(6) Sb(3) . 3.386(2) yes
I(8) Sb(2) . 2.804(2) yes
I(10) Sb(3) . 2.789(2) yes
N(1) C(1) . 1.31(2) yes
N(2) C(3) . 1.28(2) yes
N(3) C(9) . 1.32(2) yes
N(4) C(11) . 1.31(2) yes
C(1) C(4) . 1.42(3) yes
C(2) C(3) . 1.42(3) yes
C(3) C(7) . 1.51(3) yes
C(9) C(12) . 1.39(3) yes
C(10) C(11) . 1.37(2) yes
C(11) C(15) . 1.51(2) yes
O(1) N(1) . 2.690(10) yes
O(2) N(2b) 1_565 2.830(10) yes
I(1) Sb(2) . 3.305(2) yes
I(2) Sb(1) . 3.052(2) yes
I(2) Sb(3) . 3.380(2) yes
I(3) Sb(3) . 3.358(2) yes
I(5) Sb(2) . 3.280(2) yes
I(6) Sb(2) . 2.845(2) yes
I(7) Sb(2) . 2.789(2) yes
I(9) Sb(3) . 2.799(2) yes
I(11) Sb(3) . 2.802(2) yes
N(1) C(2) . 1.35(2) yes
N(2) C(4) . 1.31(2) yes
N(3) C(10) . 1.34(2) yes
N(4) C(12) . 1.38(2) yes
C(1) C(5) . 1.52(3) yes
C(2) C(6) . 1.49(3) yes
C(4) C(8) . 1.51(3) yes
C(9) C(13) . 1.53(2) yes
C(10) C(14) . 1.54(3) yes
C(12) C(16) . 1.51(3) yes
O(1) N(4) . 2.950(10) yes
O(2) N(3) . 2.750(10) yes
