#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006416.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_2006416
loop_
_publ_author_name
'Ejsmont, K.'
'Kubiak, R.'
_publ_section_title
;
 Isostructural Complexes of Diiodo(phthalocyaninato)germanium(IV) and
 Diiodo(phthalocyaninato)tin(IV)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1051
_journal_page_last               1054
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Sn I2 (C32 H16 N8)]'
_chemical_formula_structural     'see file mpci.ps'
_chemical_formula_sum            'C32 H16 I2 N8 Sn'
_chemical_formula_weight         885.031
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                73.34(3)
_cell_angle_beta                 77.20(3)
_cell_angle_gamma                87.05(3)
_cell_formula_units_Z            1
_cell_length_a                   7.618(2)
_cell_length_b                   8.551(2)
_cell_length_c                   11.602(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.80
_cell_measurement_theta_min      9.69
_cell_volume                     706.0(3)
_computing_cell_refinement       'Kuma Diffraction Software'
_computing_data_collection
'Kuma Diffraction Software (Kuma Diffraction, 1995)'
_computing_data_reduction        'Kuma Diffraction Software'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1991)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'KUMA KM--4 diffractometer'
_diffrn_measurement_method       '\w--2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8248
_diffrn_reflns_theta_max         31.06
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        <1.01
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.131
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   'empirical via \y scans (Sheldrick, 1991)'
_exptl_crystal_colour            red--violet
_exptl_crystal_density_diffrn    2.0816
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             420.0
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         '+1.11 at 0.87 \%A I1'
_refine_diff_density_min         '-1.12 at 0.73 \%A I1'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_obs   1.083
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_restrained_S_obs      1.083
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_obs          0.0300
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.3021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.0789
_refine_ls_wR_factor_obs         0.0740
_reflns_number_observed          3563
_reflns_number_total             4365
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    mu1316.cif
_[local]_cod_data_source_block   2
_cod_database_code               2006416
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
I1 0.05725(14) 0.0667(2) 0.04718(13) 0.02346(11) -0.02611(10) -0.02817(11)
Sn1 0.03870(13) 0.03325(12) 0.02205(11) -0.00363(9) -0.00229(8) -0.01307(8)
N1 0.0390(12) 0.0357(11) 0.0278(10) 0.0003(9) -0.0062(8) -0.0142(8)
N2 0.0374(11) 0.0359(10) 0.0237(9) -0.0018(8) -0.0045(8) -0.0146(8)
N3 0.0409(12) 0.0375(11) 0.0266(10) -0.0002(9) -0.0052(8) -0.0132(8)
N4 0.0416(12) 0.0343(10) 0.0265(10) -0.0052(9) -0.0017(8) -0.0135(8)
C1 0.0374(13) 0.0338(11) 0.0270(11) 0.0034(9) -0.0084(9) -0.0147(9)
C2 0.0367(13) 0.0379(12) 0.0282(11) 0.0044(10) -0.0071(9) -0.0159(9)
C3 0.052(2) 0.0448(15) 0.0364(14) 0.0009(12) -0.0094(12) -0.0225(12)
C4 0.068(2) 0.061(2) 0.041(2) -0.002(2) -0.0105(15) -0.0334(15)
C5 0.067(2) 0.062(2) 0.0271(13) 0.001(2) -0.0052(13) -0.0232(13)
C6 0.053(2) 0.047(2) 0.0272(12) 0.0020(13) -0.0041(11) -0.0160(11)
C7 0.0391(13) 0.0389(13) 0.0259(11) 0.0051(10) -0.0079(9) -0.0164(9)
C8 0.0357(12) 0.0373(12) 0.0219(10) 0.0036(9) -0.0043(9) -0.0129(9)
C9 0.0381(13) 0.0315(11) 0.0250(11) -0.0013(9) -0.0053(9) -0.0084(9)
C10 0.0388(13) 0.0317(11) 0.0261(11) 0.0015(9) -0.0088(9) -0.0066(9)
C11 0.044(2) 0.0408(14) 0.0303(13) 0.0000(11) -0.0058(11) -0.0071(11)
C12 0.052(2) 0.0394(15) 0.043(2) -0.0069(13) -0.0075(13) -0.0024(12)
C13 0.054(2) 0.0368(14) 0.051(2) -0.0073(13) -0.0122(14) -0.0075(13)
C14 0.046(2) 0.0327(12) 0.0408(15) 0.0003(11) -0.0127(12) -0.0118(11)
C15 0.0361(13) 0.0320(11) 0.0303(12) 0.0036(9) -0.0087(9) -0.0099(9)
C16 0.0377(13) 0.0321(11) 0.0287(11) -0.0013(9) -0.0066(9) -0.0132(9)
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_type_symbol
I1 0.22649(3) 0.16641(3) 0.38560(2) 0.05290(8) Uani d . 1 I
Sn1 0.5000 0.0000 0.5000 0.03076(7) Uani d S 1 Sn
N1 0.6170(3) 0.3291(3) 0.5763(2) 0.0332(4) Uani d . 1 N
N2 0.4211(3) 0.0897(3) 0.6499(2) 0.0313(4) Uani d . 1 N
N3 0.2311(3) -0.1386(3) 0.7840(2) 0.0344(4) Uani d . 1 N
N4 0.3337(3) -0.1983(3) 0.5881(2) 0.0338(4) Uani d . 1 N
C1 0.5003(4) 0.2228(3) 0.6615(2) 0.0313(5) Uani d . 1 C
C2 0.4376(4) 0.2257(3) 0.7885(2) 0.0330(5) Uani d . 1 C
C3 0.4725(5) 0.3328(4) 0.8512(3) 0.0420(6) Uani d . 1 C
C4 0.3964(5) 0.2952(5) 0.9759(3) 0.0526(8) Uani d . 1 C
C5 0.2865(5) 0.1598(5) 1.0363(3) 0.0503(8) Uani d . 1 C
C6 0.2480(5) 0.0531(4) 0.9741(3) 0.0421(6) Uani d . 1 C
C7 0.3268(4) 0.0882(3) 0.8495(2) 0.0331(5) Uani d . 1 C
C8 0.3180(4) 0.0020(3) 0.7595(2) 0.0311(5) Uani d . 1 C
C9 0.2366(4) -0.2276(3) 0.7057(2) 0.0316(5) Uani d . 1 C
C10 0.1376(4) -0.3799(3) 0.7344(2) 0.0323(5) Uani d . 1 C
C11 0.0174(4) -0.4631(4) 0.8385(3) 0.0393(6) Uani d . 1 C
C12 -0.0587(5) -0.6063(4) 0.8359(3) 0.0470(7) Uani d . 1 C
C13 -0.0152(5) -0.6621(4) 0.7330(3) 0.0479(7) Uani d . 1 C
C14 0.1058(4) -0.5789(3) 0.6276(3) 0.0392(6) Uani d . 1 C
C15 0.1835(4) -0.4363(3) 0.6297(2) 0.0325(5) Uani d . 1 C
C16 0.3097(4) -0.3195(3) 0.5364(2) 0.0319(5) Uani d . 1 C
H1 0.541(5) 0.431(5) 0.807(4) 0.050(10) Uiso d . 1 H
H2 0.426(7) 0.359(6) 1.021(5) 0.077(14) Uiso d . 1 H
H3 0.250(6) 0.135(5) 1.119(4) 0.066(13) Uiso d . 1 H
H4 0.183(5) -0.051(5) 1.017(4) 0.051(10) Uiso d . 1 H
H5 -0.012(5) -0.423(4) 0.900(3) 0.039(9) Uiso d . 1 H
H6 -0.147(6) -0.668(6) 0.916(4) 0.073(14) Uiso d . 1 H
H7 -0.071(6) -0.773(5) 0.742(4) 0.064(12) Uiso d . 1 H
H8 0.129(4) -0.613(4) 0.563(3) 0.035(9) Uiso d . 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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N4 Sn1 N4 2_656 . 180.0 ?
N4 Sn1 N2 2_656 2_656 90.06(9) ?
N4 Sn1 N2 . 2_656 89.94(9) ?
N4 Sn1 N2 2_656 . 89.94(9) ?
N4 Sn1 N2 . . 90.06(9) yes
N2 Sn1 N2 2_656 . 180.0 ?
N4 Sn1 I1 2_656 . 89.24(8) ?
N4 Sn1 I1 . . 90.76(8) yes
N2 Sn1 I1 2_656 . 87.06(7) ?
N2 Sn1 I1 . . 92.94(7) yes
N4 Sn1 I1 2_656 2_656 90.76(8) ?
N4 Sn1 I1 . 2_656 89.24(8) ?
N2 Sn1 I1 2_656 2_656 92.94(7) ?
N2 Sn1 I1 . 2_656 87.06(7) ?
I1 Sn1 I1 . 2_656 180.0 ?
C16 N1 C1 2_656 . 126.1(2) ?
C8 N2 C1 . . 111.7(2) yes
C8 N2 Sn1 . . 123.1(2) yes
C1 N2 Sn1 . . 123.3(2) yes
C8 N3 C9 . . 125.8(2) yes
C9 N4 C16 . . 112.0(2) yes
C9 N4 Sn1 . . 123.9(2) yes
C16 N4 Sn1 . . 124.0(2) yes
N1 C1 N2 . . 128.1(2) yes
N1 C1 C2 . . 125.0(2) yes
N2 C1 C2 . . 106.9(2) yes
C3 C2 C7 . . 120.8(3) yes
C3 C2 C1 . . 131.9(3) yes
C7 C2 C1 . . 107.2(2) yes
C4 C3 C2 . . 117.2(3) ?
C5 C4 C3 . . 122.1(3) ?
C4 C5 C6 . . 121.3(3) ?
C7 C6 C5 . . 116.9(3) ?
C6 C7 C2 . . 121.7(2) yes
C6 C7 C8 . . 130.9(3) yes
C2 C7 C8 . . 107.4(2) yes
N3 C8 N2 . . 128.2(2) yes
N3 C8 C7 . . 125.1(2) yes
N2 C8 C7 . . 106.7(2) yes
N3 C9 N4 . . 128.2(2) yes
N3 C9 C10 . . 124.7(2) yes
N4 C9 C10 . . 107.1(2) yes
C11 C10 C15 . . 121.8(3) yes
C11 C10 C9 . . 131.3(3) yes
C15 C10 C9 . . 106.9(2) yes
C10 C11 C12 . . 117.3(3) ?
C13 C12 C11 . . 121.3(3) ?
C12 C13 C14 . . 121.8(3) ?
C13 C14 C15 . . 117.3(3) ?
C14 C15 C10 . . 120.5(3) yes
C14 C15 C16 . . 131.6(3) yes
C10 C15 C16 . . 107.8(2) yes
N1 C16 N4 2_656 . 127.8(2) ?
N1 C16 C15 2_656 . 126.0(2) ?
N4 C16 C15 . . 106.2(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
I1 Sn1 . 2.8222(10) yes
Sn1 N4 2_656 2.044(2) ?
Sn1 N4 . 2.044(2) yes
Sn1 N2 2_656 2.056(2) ?
Sn1 N2 . 2.056(2) yes
Sn1 I1 2_656 2.8222(10) ?
N1 C16 2_656 1.327(3) yes
N1 C1 . 1.331(3) yes
N2 C8 . 1.367(3) yes
N2 C1 . 1.368(3) yes
N3 C8 . 1.329(3) yes
N3 C9 . 1.336(3) yes
N4 C9 . 1.359(3) yes
N4 C16 . 1.376(3) yes
C1 C2 . 1.452(3) yes
C2 C3 . 1.389(4) ?
C2 C7 . 1.399(4) yes
C3 C4 . 1.384(5) ?
C4 C5 . 1.381(5) ?
C5 C6 . 1.392(4) ?
C6 C7 . 1.388(4) ?
C7 C8 . 1.455(3) yes
C9 C10 . 1.455(3) yes
C10 C11 . 1.374(4) ?
C10 C15 . 1.400(4) yes
C11 C12 . 1.392(4) ?
C12 C13 . 1.378(5) ?
C13 C14 . 1.386(5) ?
C14 C15 . 1.391(4) ?
C15 C16 . 1.453(4) yes
C16 N1 2_656 1.327(3) ?