data_2003017
_journal_name_full     'Acta Crystallographica, Section B'
_journal_year     1998
_journal_volume     B54
_journal_page_first     663
_journal_page_last     670
_chemical_formula_sum     '[Zn I2 (C3 H7 N  O )2 ]'
_chemical_formula_weight     465.36
_chemical_melting_point     ?
_symmetry_cell_setting     Monoclinic
_symmetry_space_group_name_H-M     'P 21/n'
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'
_cell_length_a     13.819(3)
_cell_length_b     13.543(3)
_cell_length_c     15.559(5)
_cell_angle_alpha     90.00
_cell_angle_beta     110.29(2)
_cell_angle_gamma     90.00
_cell_volume     2731.2(12)
_cell_formula_units_Z     8
_cell_measurement_reflns_used     18
_cell_measurement_theta_min     5.40
_cell_measurement_theta_max     12.93
_cell_measurement_temperature     131(2)
_exptl_crystal_description     block
_exptl_crystal_colour     colourless
_exptl_crystal_size_max     0.44
_exptl_crystal_size_mid     0.40
_exptl_crystal_size_min     0.22
_exptl_crystal_density_diffrn     2.263
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     ?
_exptl_crystal_F_000     1728
_exptl_absorpt_coefficient_mu     6.298
_exptl_absorpt_correction_type     empirical
_exptl_absorpt_correction_T_min     0.441
_exptl_absorpt_correction_T_max     1.000
_diffrn_ambient_temperature     131(2)
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device     'Siemens P4 four-circle'
_diffrn_measurement_method     \w
_diffrn_reflns_number     5017
_diffrn_reflns_av_R_equivalents     0.0327
_diffrn_reflns_av_sigmaI/netI     0.0258
_diffrn_reflns_theta_min     2.05
_diffrn_reflns_theta_max     25.00
_diffrn_reflns_limit_h_min     0
_diffrn_reflns_limit_h_max     16
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     16
_diffrn_reflns_limit_l_min     -18
_diffrn_reflns_limit_l_max     17
_diffrn_standards_number     3
_diffrn_standards_interval_count     97
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     'No decay; steady +/-2.5'
_reflns_number_total     4804
_reflns_number_observed     3970
_reflns_observed_criterion     I>2sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0583
_refine_ls_R_factor_obs     0.0389
_refine_ls_wR_factor_all     0.2139
_refine_ls_wR_factor_obs     0.1263
_refine_ls_goodness_of_fit_all     1.122
_refine_ls_goodness_of_fit_obs     1.118
_refine_ls_restrained_S_all     1.449
_refine_ls_restrained_S_obs     0.943
_refine_ls_number_reflns     4773
_refine_ls_number_parameters     239
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     noref
_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_shift/esd_max     0.001
_refine_ls_shift/esd_mean     0.005
_refine_diff_density_max     1.836
_refine_diff_density_min     -1.581
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_extinction_coef     0.00033(12)
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_
    _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_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)