#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/08/2010854.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_2010854
loop_
_publ_author_name
'Harrison, William T. A.'
'Howie, R. Alan'
'Skakle, Janet'
'Wardell, James L.'
_publ_section_title
;
 Bis(tetraethylammonium) tetraiodozincate at 150 and 301K
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e124
_journal_page_last               e125
_journal_paper_doi               10.1107/S0108270100003383
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '(C8 H20 N)2 [Zn I4]'
_chemical_formula_moiety         '(C8 H20 N +)2, (I4 Zn 2-)'
_chemical_formula_sum            'C16 H40 I4 N2 Zn'
_chemical_formula_weight         833.47
_chemical_name_systematic
;
 bis(tetraethylammonium) tertraiodozincate
;
_space_group_IT_number           113
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2ab'
_symmetry_space_group_name_H-M   'P -4 21 m'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8199(6)
_cell_length_b                   13.8199(6)
_cell_length_c                   14.8975(7)
_cell_measurement_reflns_used    4735
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      21.71
_cell_measurement_theta_min      2.49
_cell_volume                     2845.3(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'starting parameters from G&F'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       φ-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  .081
_diffrn_reflns_av_sigmaI/netI    .0417
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17580
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.37
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.206
_exptl_absorpt_correction_T_max  .413
_exptl_absorpt_correction_T_min  .196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.946
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .28
_exptl_crystal_size_min          .17
_refine_diff_density_max         1.39
_refine_diff_density_min         -.67
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   .29(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .993
_refine_ls_R_factor_all          .075
_refine_ls_R_factor_gt           .049
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0828P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .135
_reflns_number_gt                1825
_reflns_number_total             2678
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            qa0237.cif
_cod_data_source_block           301K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0828P)^2^] where P = (Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.0828P)^2^]
where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2010854
_cod_database_fobs_code          2010854
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-y+1/2, -x+1/2, z'
'-y, x, -z'
'y, -x, -z'
'y+1/2, x+1/2, z'
'-x+1/2, y+1/2, -z'
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
Zn1 .74758(8) .75242(8) .72848(10) .0587(4) Uani d S 1 . . Zn
I1 .57305(6) .70492(8) .78081(7) .1031(4) Uani d . 1 . . I
I2 .86988(7) .63012(7) .79847(9) .0986(4) Uani d S 1 . . I
I3 .75521(7) .74479(7) .55304(7) .0839(4) Uani d S 1 . . I
N1 .5000 .5000 .5000 .060(4) Uani d S 1 . . N
C1 .5387(10) .4186(11) .5571(11) .093(4) Uani d . 1 . . C
H1A .5657 .3691 .5183 .111 Uiso calc R 1 . . H
H1B .4857 .3899 .5905 .111 Uiso calc R 1 . . H
C2 .6178(10) .4528(12) .6240(10) .102(5) Uani d . 1 . . C
H2A .6666 .4884 .5922 .154 Uiso calc R 1 . . H
H2B .6466 .3975 .6524 .154 Uiso calc R 1 . . H
H2C .5890 .4936 .6688 .154 Uiso calc R 1 . . H
N2 1.0000 .5000 .4804(17) .085(6) Uani d S 1 . . N
C3 .917(2) .491(2) .5421(17) .111(9) Uani d P .50 . . C
H3A .8592 .4865 .5053 .134 Uiso calc PR .50 . . H
H3B .9122 .5520 .5747 .134 Uiso calc PR .50 . . H
C4 .9116(12) .4116(12) .6103(16) .121(8) Uani d S 1 . . C
H4A .9483 .3570 .5896 .182 Uiso calc PR .50 . . H
H4B .8453 .3928 .6187 .182 Uiso calc PR .50 . . H
H4C .9377 .4340 .6663 .182 Uiso calc PR .50 . . H
C5 1.006(2) .417(2) .427(2) .126(11) Uani d P .50 . . C
H5A .9484 .4149 .3904 .151 Uiso calc PR .50 . . H
H5B 1.0040 .3618 .4670 .151 Uiso calc PR .50 . . H
C6 1.0960(18) .4040(18) .3633(16) .172(14) Uani d S 1 . . C
H6A 1.0891 .3449 .3301 .258 Uiso calc PR .50 . . H
H6B 1.1542 .4015 .3985 .258 Uiso calc PR .50 . . H
H6C 1.0994 .4575 .3223 .258 Uiso calc PR .50 . . H
N3 .7905(6) .2905(6) .9198(8) .070(3) Uani d S 1 . . N
C7 .8311(17) .3311(17) 1.0025(17) .143(10) Uani d S 1 . . C
H7A .8587 .2787 1.0374 .171 Uiso calc PR .50 . . H
H7B .7787 .3587 1.0374 .171 Uiso calc PR .50 . . H
C8 .9103(13) .4103(13) .989(2) .182(15) Uani d S 1 . . C
H8A .9325 .4325 1.0467 .273 Uiso calc SR 1 . . H
H8B .8835 .4637 .9563 .273 Uiso calc PR .50 . . H
H8C .9637 .3835 .9563 .273 Uiso calc PR .50 . . H
C9 .7152(12) .2152(12) .953(2) .130(9) Uani d S 1 . . C
H9A .6671 .2474 .9898 .156 Uiso calc PR .50 . . H
H9B .7474 .1671 .9898 .156 Uiso calc PR .50 . . H
C10 .6635(13) .1635(13) .871(3) .188(18) Uani d S 1 . . C
H10A .6174 .1174 .8937 .282 Uiso calc SR 1 . . H
H10B .7110 .1308 .8354 .282 Uiso calc PR .50 . . H
H10C .6308 .2110 .8354 .282 Uiso calc PR .50 . . H
C11 .7409(15) .3657(14) .8653(11) .134(6) Uani d . 1 . . C
H11A .7102 .3343 .8145 .161 Uiso calc R 1 . . H
H11B .7895 .4095 .8418 .161 Uiso calc R 1 . . H
C12 .6639(14) .4259(14) .9151(16) .143(7) Uani d . 1 . . C
H12A .6157 .3835 .9397 .214 Uiso calc R 1 . . H
H12B .6339 .4701 .8739 .214 Uiso calc R 1 . . H
H12C .6941 .4616 .9628 .214 Uiso calc R 1 . . H
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'
I I -.4742 1.8119 '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'
Zn Zn .2839 1.4301 '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
I2 Zn1 I3 . . 110.30(7)
I2 Zn1 I1 . 4_665 108.39(5)
I3 Zn1 I1 . 4_665 108.92(5)
I2 Zn1 I1 . . 108.39(5)
I3 Zn1 I1 . . 108.92(5)
I1 Zn1 I1 4_665 . 111.92(7)
C1 N1 C1 5_656 6_566 111.4(12)
C1 N1 C1 5_656 . 108.5(6)
C1 N1 C1 6_566 . 108.5(6)
C1 N1 C1 5_656 2_665 108.5(6)
C1 N1 C1 6_566 2_665 108.5(6)
C1 N1 C1 . 2_665 111.4(12)
N1 C1 C2 . . 112.6(11)
C5 N2 C5 2_765 7_545 65(3)
C5 N2 C5 2_765 . 111(3)
C5 N2 C5 7_545 . 77(3)
C5 N2 C5 2_765 4_665 77(3)
C5 N2 C5 7_545 4_665 111(3)
C5 N2 C5 . 4_665 65(3)
C5 N2 C3 2_765 4_665 73.8(19)
C5 N2 C3 7_545 4_665 111.9(17)
C5 N2 C3 . 4_665 171(2)
C5 N2 C3 4_665 4_665 109.6(18)
C5 N2 C3 2_765 . 111.9(17)
C5 N2 C3 7_545 . 73.8(19)
C5 N2 C3 . . 109.6(18)
C5 N2 C3 4_665 . 171(2)
C3 N2 C3 4_665 . 75(3)
C5 N2 C3 2_765 7_545 171(2)
C5 N2 C3 7_545 7_545 109.6(18)
C5 N2 C3 . 7_545 73.8(19)
C5 N2 C3 4_665 7_545 111.9(17)
C3 N2 C3 4_665 7_545 103(3)
C3 N2 C3 . 7_545 59(2)
C5 N2 C3 2_765 2_765 109.6(18)
C5 N2 C3 7_545 2_765 171(2)
C5 N2 C3 . 2_765 111.9(17)
C5 N2 C3 4_665 2_765 73.8(19)
C3 N2 C3 4_665 2_765 59(2)
C3 N2 C3 . 2_765 103(3)
C3 N2 C3 7_545 2_765 75(3)
N2 C3 C4 . . 121(2)
N2 C5 C6 . . 119(3)
C7 N3 C11 . 7_545 111.6(12)
C7 N3 C11 . . 111.6(12)
C11 N3 C11 7_545 . 110.3(17)
C7 N3 C9 . . 104.2(18)
C11 N3 C9 7_545 . 109.5(11)
C11 N3 C9 . . 109.5(11)
N3 C7 C8 . . 115(2)
N3 C9 C10 . . 111(2)
N3 C11 C12 . . 115.7(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
Zn1 I2 . 2.608(2) ?
Zn1 I3 . 2.6178(18) ?
Zn1 I1 4_665 2.6185(12) ?
Zn1 I1 . 2.6185(12) ?
N1 C1 5_656 1.508(14) ?
N1 C1 6_566 1.508(14) ?
N1 C1 . 1.508(14) ?
N1 C1 2_665 1.508(14) ?
C1 C2 . 1.55(2) ?
N2 C5 2_765 1.39(3) ?
N2 C5 7_545 1.39(3) ?
N2 C5 . 1.39(3) ?
N2 C5 4_665 1.39(3) ?
N2 C3 4_665 1.48(3) ?
N2 C3 . 1.48(3) ?
N2 C3 7_545 1.48(3) ?
N2 C3 2_765 1.48(3) ?
C3 C4 . 1.50(3) ?
C5 C6 . 1.58(4) ?
N3 C7 . 1.47(3) ?
N3 C11 7_545 1.486(17) ?
N3 C11 . 1.486(17) ?
N3 C9 . 1.55(3) ?
C7 C8 . 1.56(4) ?
C9 C10 . 1.58(4) ?
C11 C12 . 1.54(2) ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
C1 N1 C1 C2 5_656 63.3(7)
C1 N1 C1 C2 6_566 -175.5(13)
C1 N1 C1 C2 2_665 -56.1(10)
C5 N2 C3 C4 2_765 -176(2)
C5 N2 C3 C4 7_545 131(3)
C5 N2 C3 C4 . 61(3)
C5 N2 C3 C4 4_665 10(17)
C3 N2 C3 C4 4_665 -111(2)
C3 N2 C3 C4 7_545 5(3)
C3 N2 C3 C4 2_765 -58(2)
C5 N2 C5 C6 2_765 63(3)
C5 N2 C5 C6 7_545 119(2)
C5 N2 C5 C6 4_665 -1(4)
C3 N2 C5 C6 4_665 -55(17)
C3 N2 C5 C6 . -173(3)
C3 N2 C5 C6 7_545 -125(3)
C3 N2 C5 C6 2_765 -60(4)
C11 N3 C7 C8 7_545 62.0(11)
C11 N3 C7 C8 . -62.0(11)
C9 N3 C7 C8 . 180.000(2)
C7 N3 C9 C10 . 180.0000(10)
C11 N3 C9 C10 7_545 -60.5(11)
C11 N3 C9 C10 . 60.5(11)
C7 N3 C11 C12 . -53(2)
C11 N3 C11 C12 7_545 -177.5(11)
C9 N3 C11 C12 . 62(2)
