#------------------------------------------------------------------------------
#$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $
#$Revision: 91933 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/30/2003017.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_2003017
loop_
_publ_author_name
'Edwards, R. A.'
'Easteal, A. J.'
'Gladkikh, O. P.'
'Robinson, W. T.'
'Turnbull, M. M.'
'Wilkins, C. J.'
_publ_section_title
;
 A Reversible Non-disruptive Phase Transition Shown by the Zinc Iodide
 Dimethylformamide Complex ZnI~2~(dmf)~2~
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              663
_journal_page_last               670
_journal_volume                  54
_journal_year                    1998
_chemical_formula_sum            'C6 H14 I2 N2 O2 Zn'
_chemical_formula_weight         465.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 110.29(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.819(3)
_cell_length_b                   13.543(3)
_cell_length_c                   15.559(5)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    131(2)
_cell_measurement_theta_max      12.93
_cell_measurement_theta_min      5.40
_cell_volume                     2731.2(13)
_computing_cell_refinement       'XSCANS (Siemens, 1989)'
_computing_data_collection       'XSCANS (Siemens, 1989)'
_computing_data_reduction        'XPREP (Sheldrick, 1993)'
_computing_molecular_graphics    'SHELXL93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      131(2)
_diffrn_measurement_device       'Siemens P4 four-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5017
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        'No decay; steady +/-2.5'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.298
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.441
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.263
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.836
_refine_diff_density_min         -1.581
_refine_ls_extinction_coef       0.00033(12)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.122
_refine_ls_goodness_of_fit_obs   1.118
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.449
_refine_ls_restrained_S_obs      0.943
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_obs          0.0389
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w=1/[s^2^(Fo^2^)+( 0.1015P)^2^+24.2896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.2139
_refine_ls_wR_factor_obs         0.1263
_reflns_number_observed          3970
_reflns_number_total             4804
_reflns_observed_criterion       I>2sigma(I)
_[local]_cod_data_source_file    mu0321.cif
_[local]_cod_data_source_block   LT
_[local]_cod_cif_authors_sg_H-M  'P 21/n'
_[local]_cod_chemical_formula_sum_orig '[Zn I2 (C3 H7 N  O )2 ]'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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        2731.2(12)
_cod_database_code               2003017
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Zn 0.0195(6) 0.0219(6) 0.0160(6) -0.0006(5) 0.0069(5) -0.0006(5)
Zn' 0.0222(6) 0.0211(6) 0.0165(6) 0.0038(5) 0.0092(5) 0.0027(5)
I2 0.0187(4) 0.0371(4) 0.0177(4) 0.0012(3) 0.0048(3) -0.0018(3)
I2' 0.0235(4) 0.0317(4) 0.0182(4) 0.0017(3) 0.0041(3) 0.0008(3)
I1 0.0229(4) 0.0227(4) 0.0259(4) -0.0011(3) 0.0038(3) -0.0036(3)
I1' 0.0316(4) 0.0226(4) 0.0256(4) 0.0045(3) 0.0106(3) 0.0075(3)
O1 0.024(4) 0.019(3) 0.024(4) -0.003(3) 0.007(3) 0.007(3)
O1' 0.021(4) 0.027(4) 0.027(4) 0.002(3) 0.010(3) -0.012(3)
O2 0.035(4) 0.022(4) 0.025(4) -0.004(3) 0.018(3) -0.007(3)
O2' 0.022(4) 0.024(4) 0.030(4) 0.006(3) 0.015(3) 0.011(3)
C1 0.020(5) 0.027(5) 0.016(5) -0.003(4) 0.004(4) 0.006(4)
C1' 0.010(4) 0.031(5) 0.017(5) 0.003(4) 0.009(4) 0.007(4)
C4 0.017(5) 0.026(5) 0.024(6) -0.003(4) 0.009(4) 0.002(4)
C4' 0.025(6) 0.034(6) 0.034(6) 0.000(5) 0.021(5) 0.003(5)
C2 0.023(6) 0.038(7) 0.059(9) -0.012(5) 0.015(6) 0.010(6)
C2' 0.032(6) 0.040(7) 0.052(8) 0.011(5) 0.033(6) -0.007(6)
C3 0.025(6) 0.037(6) 0.031(6) 0.011(5) 0.009(5) 0.007(5)
C3' 0.040(7) 0.035(6) 0.021(6) -0.011(5) 0.011(5) 0.002(5)
C5 0.034(6) 0.029(6) 0.037(7) 0.013(5) 0.024(5) -0.004(5)
C5' 0.083(11) 0.037(7) 0.038(8) 0.013(7) 0.042(8) 0.022(6)
C6 0.046(7) 0.027(6) 0.039(7) 0.013(5) 0.030(6) 0.000(5)
C6' 0.012(5) 0.048(7) 0.023(6) -0.012(5) 0.005(4) 0.002(5)
N1 0.015(4) 0.030(5) 0.026(5) -0.002(4) 0.010(4) -0.012(4)
N1' 0.027(5) 0.029(5) 0.017(4) -0.004(4) 0.010(4) 0.010(4)
N2 0.019(4) 0.025(4) 0.018(4) 0.003(4) 0.001(3) 0.002(4)
N2' 0.032(5) 0.017(4) 0.020(4) 0.005(4) 0.019(4) 0.003(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_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Zn 0.23024(9) 0.40636(9) 0.25162(8) 0.0190(3) Uani d . 1 . Zn
Zn' -0.24541(9) 0.39954(9) 0.24954(8) 0.0193(3) Uani d . 1 . Zn
I2 0.04123(5) 0.42582(5) 0.15298(5) 0.0249(2) Uani d . 1 . I
I2' -0.07190(5) 0.38119(5) 0.37812(5) 0.0253(2) Uani d . 1 . I
I1 0.31854(5) 0.55535(5) 0.34738(5) 0.0250(2) Uani d . 1 . I
I1' -0.30826(5) 0.55462(5) 0.15672(5) 0.0264(2) Uani d . 1 . I
O1 0.2499(5) 0.2890(5) 0.3350(5) 0.022(2) Uani d . 1 . O
O1' -0.2643(5) 0.2874(5) 0.1627(5) 0.025(2) Uani d . 1 . O
O2 0.3199(6) 0.3591(5) 0.1822(5) 0.025(2) Uani d . 1 . O
O2' -0.3528(5) 0.3656(5) 0.3045(5) 0.024(2) Uani d . 1 . O
C1 0.1735(8) 0.2395(8) 0.3407(7) 0.022(2) Uani d . 1 . C
H1 0.1048(8) 0.2593(8) 0.3041(7) 0.02(3) Uiso d R 1 . H
C1' -0.1895(7) 0.2354(8) 0.1581(7) 0.018(2) Uani d . 1 . C
H1' -0.1212(7) 0.2525(8) 0.1977(7) 0.04(4) Uiso d R 1 . H
C4 0.3614(7) 0.2781(8) 0.1924(7) 0.022(2) Uani d . 1 . C
H4 0.3440(7) 0.2304(8) 0.2294(7) 0.027 Uiso d R 1 . H
C4' -0.3381(8) 0.2972(9) 0.3602(8) 0.029(2) Uani d . 1 . C
H4' -0.2777(8) 0.2570(9) 0.3712(8) 0.06(5) Uiso d R 1 . H
C2 0.0960(9) 0.1048(9) 0.3927(10) 0.040(3) Uani d . 1 . C
H2A 0.1002(9) 0.0954(9) 0.4563(10) 0.048 Uiso d R 1 . H
H2B 0.0980(9) 0.0404(9) 0.3646(10) 0.048 Uiso d R 1 . H
H2C 0.0314(9) 0.1386(9) 0.3584(10) 0.048 Uiso d R 1 . H
C2' -0.1084(9) 0.1018(9) 0.1076(10) 0.036(3) Uani d . 1 . C
H2A' -0.1122(9) 0.0843(9) 0.0454(10) 0.044 Uiso d R 1 . H
H2B' -0.1063(9) 0.0415(9) 0.1429(10) 0.044 Uiso d R 1 . H
H2C' -0.0460(9) 0.1407(9) 0.1373(10) 0.044 Uiso d R 1 . H
C3 0.2877(8) 0.1246(9) 0.4494(8) 0.031(3) Uani d . 1 . C
H3A 0.3094(8) 0.0758(9) 0.4133(8) 0.037 Uiso d R 1 . H
H3B 0.2832(8) 0.0932(9) 0.5046(8) 0.037 Uiso d R 1 . H
H3C 0.3381(8) 0.1785(9) 0.4670(8) 0.037 Uiso d R 1 . H
C3' -0.3004(9) 0.1268(9) 0.0448(8) 0.032(3) Uani d . 1 . C
H3A' -0.3111(9) 0.0593(9) 0.0623(8) 0.038 Uiso d R 1 . H
H3B' -0.3042(9) 0.1275(9) -0.0193(8) 0.038 Uiso d R 1 . H
H3C' -0.3539(9) 0.1701(9) 0.0520(8) 0.038 Uiso d R 1 . H
C5 0.4737(9) 0.1528(8) 0.1641(8) 0.030(3) Uani d . 1 . C
H5A 0.5489(9) 0.1596(8) 0.1895(8) 0.037 Uiso d R 1 . H
H5B 0.4540(9) 0.1181(8) 0.1053(8) 0.037 Uiso d R 1 . H
H5C 0.4500(9) 0.1150(8) 0.2068(8) 0.037 Uiso d R 1 . H
C5' -0.3773(12) 0.1932(10) 0.4711(9) 0.048(4) Uani d . 1 . C
H5A' -0.4326(12) 0.1892(10) 0.4968(9) 0.057 Uiso d R 1 . H
H5B' -0.3111(12) 0.2033(10) 0.5206(9) 0.057 Uiso d R 1 . H
H5C' -0.3748(12) 0.1316(10) 0.4388(9) 0.057 Uiso d R 1 . H
C6 0.4522(10) 0.3186(9) 0.0891(9) 0.033(3) Uani d . 1 . C
H6A 0.4816(10) 0.2804(9) 0.0505(9) 0.040 Uiso d R 1 . H
H6B 0.5034(10) 0.3663(9) 0.1255(9) 0.040 Uiso d R 1 . H
H6C 0.3907(10) 0.3538(9) 0.0502(9) 0.040 Uiso d R 1 . H
C6' -0.4853(7) 0.3415(9) 0.4018(8) 0.028(2) Uani d . 1 . C
H6A' -0.4716(7) 0.3728(9) 0.4617(8) 0.034 Uiso d R 1 . H
H6B' -0.5483(7) 0.3018(9) 0.3863(8) 0.034 Uiso d R 1 . H
H6C' -0.4941(7) 0.3926(9) 0.3551(8) 0.034 Uiso d R 1 . H
N1 0.1866(6) 0.1630(7) 0.3945(6) 0.023(2) Uani d . 1 . N
N1' -0.1994(7) 0.1617(6) 0.1034(6) 0.024(2) Uani d . 1 . N
N2 0.4275(6) 0.2533(6) 0.1509(6) 0.022(2) Uani d . 1 . N
N2' -0.3966(7) 0.2767(6) 0.4071(6) 0.021(2) Uani d . 1 . N
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'
Zn Zn .2839 1.4301 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1 Zn O2 97.1(3)
O1 Zn I2 110.6(2)
O2 Zn I2 113.8(2)
O1 Zn I1 108.5(2)
O2 Zn I1 107.9(2)
I2 Zn I1 116.95(5)
O1' Zn' O2' 99.9(3)
O1' Zn' I1' 108.0(2)
O2' Zn' I1' 106.0(2)
O1' Zn' I2' 109.0(2)
O2' Zn' I2' 106.1(2)
I1' Zn' I2' 125.00(5)
C1 O1 Zn 122.0(6)
C1' O1' Zn' 122.9(7)
C4 O2 Zn 124.4(7)
C4' O2' Zn' 120.3(7)
O1 C1 N1 121.7(9)
O1' C1' N1' 124.3(9)
O2 C4 N2 122.2(10)
O2' C4' N2' 125.0(10)
C1 N1 C3 123.5(9)
C1 N1 C2 119.0(9)
C3 N1 C2 117.1(10)
C1' N1' C3' 121.7(9)
C1' N1' C2' 120.2(9)
C3' N1' C2' 117.7(10)
C4 N2 C6 122.2(9)
C4 N2 C5 119.9(9)
C6 N2 C5 117.8(9)
C4' N2' C5' 123.1(10)
C4' N2' C6' 120.5(9)
C5' N2' C6' 116.3(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Zn O1 2.009(7)
Zn O2 2.010(7)
Zn I2 2.5431(15)
Zn I1 2.5532(14)
Zn' O1' 1.989(7)
Zn' O2' 2.006(7)
Zn' I1' 2.5260(14)
Zn' I2' 2.547(2)
O1 C1 1.281(12)
O1' C1' 1.273(12)
O2 C4 1.223(12)
O2' C4' 1.237(13)
C1 N1 1.304(13)
C1' N1' 1.287(14)
C4 N2 1.331(13)
C4' N2' 1.292(13)
C2 N1 1.471(13)
C2' N1' 1.479(13)
C3 N1 1.457(14)
C3' N1' 1.456(14)
C5 N2 1.487(13)
C5' N2' 1.469(14)
C6 N2 1.432(15)
C6' N2' 1.487(14)
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
O2 Zn O1 C1 -124.9(8)
O1 Zn O2 C4 4.5(8)
I1 Zn O1 C1 123.5(7)
I2 Zn O1 C1 -6.1(8)
I1 Zn O2 C4 116.6(8)
I2 Zn O2 C4 -111.9(8)
O1 C1 N1 C2 -175.4(10)
O1 C1 N1 C3 -2.6(16)
O2 C4 N2 C5 -178.4(10)
O2 C4 N2 C6 -2.0(16)
Zn O1 C1 N1 179.6(7)
Zn O2 C4 N2 -173.8(7)
O2' Zn' O1' C1' -130.7(8)
O1' Zn' O2' C4' 74.2(9)
I1' Zn' O1' C1' 118.8(7)
I2' Zn' O1' C1' -19.7(8)
I1' Zn' O2' C4' -173.7(8)
I2' Zn' O2' C4' -39.0(9)
O1' C1' N1' C2' -175.9(10)
O1' C1' N1' C3' -4.1(15)
O2' C4' N2' C5' 178.6(12)
O2' C4' N2' C6' -4.7(18)
Zn' O1' C1' N1' 179.2(7)
Zn' O2' C4' N2' 171.7(9)
_journal_paper_doi 10.1107/S0108768198000536