#------------------------------------------------------------------------------
#$Date: 2019-10-28 09:23:29 +0200 (Mon, 28 Oct 2019) $
#$Revision: 219800 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/01/41/2014181.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_2014181
loop_
_publ_author_name
'Janczak, Jan'
_publ_section_title
;
 Iodo[phthalocyaninato(2--)]manganese(III) bridged by a neutral I₂
 molecule
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m330
_journal_page_last               m332
_journal_paper_doi               10.1107/S0108270104012387
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '2[Mn (C32 H16 Mn N8) I] , I2'
_chemical_formula_moiety         '2(C32 H16 I Mn N8) , I2'
_chemical_formula_sum            'C64 H32 I4 Mn2 N16'
_chemical_formula_weight         1642.54
_chemical_melting_point          'loses the I~2~ molecule'
_chemical_name_common
;
manganium phthalocyanine
;
_chemical_name_systematic
;
Iodo[phthalocyaninato(2-)]manganese(III) hemi(diiodine)
;
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                102.11(2)
_cell_angle_beta                 91.61(2)
_cell_angle_gamma                96.81(2)
_cell_formula_units_Z            1
_cell_length_a                   8.447(2)
_cell_length_b                   13.051(2)
_cell_length_c                   13.218(2)
_cell_measurement_reflns_used    2544
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2.97
_cell_volume                     1412.6(5)
_computing_cell_refinement       'KM-4 CCD Software'
_computing_data_collection       'KM-4 CCD Software (Kuma, 2001)'
_computing_data_reduction        'KM-4 CCD Software'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Kuma KM-4 with CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16124
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.97
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.692
_exptl_absorpt_correction_T_max  0.6559
_exptl_absorpt_correction_T_min  0.5632
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'face-indexed (SHELXTL; Sheldrick, 1990)'
_exptl_crystal_colour            black-violet
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_density_meas      1.93
_exptl_crystal_density_method    'flotation in a mixture of CHBr~3~/CHCl~3~'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.817
_refine_diff_density_min         -1.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0162P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                4580
_reflns_number_total             6769
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gg1221.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-10-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C32 H16 I2 Mn N8'
_cod_original_formula_weight         821.27
_cod_original_formula_moiety         'C32 H16 I Mn N8 , 0.5I2'
_cod_original_formula_iupac          '[Mn (C32 H16 Mn N8) I] , 0.5I2'
_cod_original_formula_units_Z            2
_cod_database_code               2014181
_cod_database_fobs_code          2014181
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
_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
I1 0.07453(5) 0.19823(3) 0.85243(3) 0.05760(14) Uani d . 1 . . I
Mn1 0.34004(10) 0.33739(6) 0.84499(6) 0.0442(2) Uani d . 1 . . Mn
I2 0.02352(6) 0.05696(4) 0.60189(4) 0.1008(2) Uani d . 1 . . I
N1 0.4907(5) 0.2497(3) 0.8913(3) 0.0432(12) Uani d . 1 . . N
N2 0.4788(5) 0.3026(3) 1.0777(3) 0.0476(13) Uani d . 1 . . N
N3 0.3392(5) 0.4156(3) 0.9896(3) 0.0430(12) Uani d . 1 . . N
N4 0.1817(5) 0.5554(3) 0.9678(3) 0.0481(13) Uani d . 1 . . N
N5 0.2406(5) 0.4512(3) 0.8013(3) 0.0428(12) Uani d . 1 . . N
N6 0.2595(5) 0.4001(3) 0.6138(3) 0.0492(13) Uani d . 1 . . N
N7 0.3941(5) 0.2860(3) 0.7021(3) 0.0396(12) Uani d . 1 . . N
N8 0.5606(5) 0.1502(3) 0.7252(4) 0.0485(13) Uani d . 1 . . N
C1 0.5602(6) 0.1695(4) 0.8259(5) 0.0447(15) Uani d . 1 . . C
C2 0.6335(6) 0.1079(4) 0.8905(5) 0.0468(16) Uani d . 1 . . C
C3 0.7208(7) 0.0210(4) 0.8640(5) 0.0631(19) Uani d . 1 . . C
H3 0.7398 -0.0076 0.7955 0.076 Uiso calc R 1 . . H
C4 0.7757(7) -0.0186(4) 0.9440(5) 0.069(2) Uani d . 1 . . C
H4 0.8329 -0.0762 0.9299 0.083 Uiso calc R 1 . . H
C5 0.7484(7) 0.0244(4) 1.0441(5) 0.0604(18) Uani d . 1 . . C
H5 0.7858 -0.0064 1.0960 0.072 Uiso calc R 1 . . H
C6 0.6668(7) 0.1126(4) 1.0730(5) 0.0606(18) Uani d . 1 . . C
H6 0.6513 0.1413 1.1421 0.073 Uiso calc R 1 . . H
C7 0.6131(6) 0.1530(4) 0.9969(4) 0.0417(15) Uani d . 1 . . C
C8 0.5189(6) 0.2415(4) 0.9921(5) 0.0425(15) Uani d . 1 . . C
C9 0.3984(6) 0.3848(4) 1.0771(4) 0.0423(15) Uani d . 1 . . C
C10 0.3558(6) 0.4535(4) 1.1685(4) 0.0451(16) Uani d . 1 . . C
C11 0.3862(6) 0.4564(4) 1.2763(4) 0.0423(15) Uani d . 1 . . C
H11 0.4482 0.4096 1.2974 0.051 Uiso calc R 1 . . H
C12 0.3218(7) 0.5296(4) 1.3474(5) 0.0628(19) Uani d . 1 . . C
H12 0.3398 0.5322 1.4177 0.075 Uiso calc R 1 . . H
C13 0.2260(7) 0.6032(4) 1.3153(5) 0.0627(19) Uani d . 1 . . C
H13 0.1819 0.6519 1.3648 0.075 Uiso calc R 1 . . H
C14 0.1998(6) 0.6014(4) 1.2101(4) 0.0513(17) Uani d . 1 . . C
H14 0.1438 0.6510 1.1889 0.062 Uiso calc R 1 . . H
C15 0.2575(6) 0.5258(4) 1.1398(4) 0.0470(16) Uani d . 1 . . C
C16 0.2560(6) 0.5018(4) 1.0238(4) 0.0424(15) Uani d . 1 . . C
C17 0.1805(6) 0.5339(4) 0.8638(4) 0.0448(15) Uani d . 1 . . C
C18 0.1175(7) 0.5986(4) 0.7991(4) 0.0528(17) Uani d . 1 . . C
C19 0.0449(7) 0.6931(4) 0.8234(4) 0.0575(18) Uani d . 1 . . C
H19 0.0252 0.7228 0.8915 0.069 Uiso calc R 1 . . H
C20 0.0046(7) 0.7395(4) 0.7435(5) 0.068(2) Uani d . 1 . . C
H20 -0.0398 0.8025 0.7578 0.081 Uiso calc R 1 . . H
C21 0.0298(7) 0.6928(4) 0.6418(5) 0.0598(18) Uani d . 1 . . C
H21 -0.0025 0.7246 0.5892 0.072 Uiso calc R 1 . . H
C22 0.0994(6) 0.6029(4) 0.6154(4) 0.0525(17) Uani d . 1 . . C
H22 0.1197 0.5742 0.5472 0.063 Uiso calc R 1 . . H
C23 0.1387(6) 0.5561(4) 0.6978(4) 0.0484(16) Uani d . 1 . . C
C24 0.2166(7) 0.4614(4) 0.6992(5) 0.0496(16) Uani d . 1 . . C
C25 0.3394(7) 0.3182(4) 0.6133(4) 0.0494(16) Uani d . 1 . . C
C26 0.3943(7) 0.2569(4) 0.5222(5) 0.0499(16) Uani d . 1 . . C
C27 0.3861(7) 0.2604(4) 0.4184(5) 0.066(2) Uani d . 1 . . C
H27 0.3269 0.3082 0.3966 0.080 Uiso calc R 1 . . H
C28 0.4632(8) 0.1951(4) 0.3475(5) 0.070(2) Uani d . 1 . . C
H28 0.4532 0.1970 0.2777 0.084 Uiso calc R 1 . . H
C29 0.5578(8) 0.1248(4) 0.3798(5) 0.076(2) Uani d . 1 . . C
H29 0.6093 0.0801 0.3309 0.092 Uiso calc R 1 . . H
C30 0.5751(7) 0.1215(4) 0.4845(5) 0.0599(18) Uani d . 1 . . C
H30 0.6397 0.0759 0.5053 0.072 Uiso calc R 1 . . H
C31 0.4954(6) 0.1867(4) 0.5574(4) 0.0457(15) Uani d . 1 . . C
C32 0.4893(7) 0.2043(4) 0.6664(5) 0.0503(17) Uani d . 1 . . C
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'
Mn Mn 0.3368 0.7283 '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'
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_3
_geom_angle
_geom_angle_publ_flag
N7 Mn1 N5 . 89.51(17) y
N7 Mn1 N3 . 164.40(17) y
N5 Mn1 N3 . 88.61(17) y
N7 Mn1 N1 . 89.30(17) y
N5 Mn1 N1 . 165.03(17) y
N3 Mn1 N1 . 88.54(17) y
N7 Mn1 I1 . 99.69(12) y
N5 Mn1 I1 . 100.08(12) y
N3 Mn1 I1 . 95.89(12) y
N1 Mn1 I1 . 94.83(12) y
I1 I2 I2 2_556 178.97(3) y
C8 N1 C1 . 108.2(4) ?
C8 N1 Mn1 . 125.4(3) ?
C1 N1 Mn1 . 125.1(4) ?
C8 N2 C9 . 122.7(5) ?
C16 N3 C9 . 107.8(4) ?
C16 N3 Mn1 . 125.3(3) ?
C9 N3 Mn1 . 126.1(3) ?
C16 N4 C17 . 122.2(4) ?
C17 N5 C24 . 107.2(4) ?
C17 N5 Mn1 . 127.2(4) ?
C24 N5 Mn1 . 125.6(3) ?
C24 N6 C25 . 124.0(5) ?
C25 N7 C32 . 106.3(4) ?
C25 N7 Mn1 . 126.9(3) ?
C32 N7 Mn1 . 126.6(4) ?
C1 N8 C32 . 124.0(5) ?
N8 C1 N1 . 127.6(5) ?
N8 C1 C2 . 124.1(5) ?
N1 C1 C2 . 108.2(5) ?
C3 C2 C7 . 120.1(5) ?
C3 C2 C1 . 131.0(5) ?
C7 C2 C1 . 108.8(5) ?
C4 C3 C2 . 116.6(5) ?
C4 C3 H3 . 121.7 ?
C2 C3 H3 . 121.7 ?
C5 C4 C3 . 121.3(5) ?
C5 C4 H4 . 119.4 ?
C3 C4 H4 . 119.4 ?
C4 C5 C6 . 123.4(6) ?
C4 C5 H5 . 118.3 ?
C6 C5 H5 . 118.3 ?
C7 C6 C5 . 116.4(6) ?
C7 C6 H6 . 121.8 ?
C5 C6 H6 . 121.8 ?
C6 C7 C2 . 122.0(5) ?
C6 C7 C8 . 134.2(5) ?
C2 C7 C8 . 103.7(5) ?
N2 C8 N1 . 128.2(5) ?
N2 C8 C7 . 120.7(5) ?
N1 C8 C7 . 111.1(5) ?
N2 C9 N3 . 126.5(5) ?
N2 C9 C10 . 124.1(5) ?
N3 C9 C10 . 109.4(4) ?
C9 C10 C15 . 109.3(5) ?
C9 C10 C11 . 131.8(5) ?
C15 C10 C11 . 118.8(5) ?
C12 C11 C10 . 118.4(5) ?
C12 C11 H11 . 120.8 ?
C10 C11 H11 . 120.8 ?
C11 C12 C13 . 121.2(6) ?
C11 C12 H12 . 119.4 ?
C13 C12 H12 . 119.4 ?
C14 C13 C12 . 120.1(5) ?
C14 C13 H13 . 120.0 ?
C12 C13 H13 . 120.0 ?
C15 C14 C13 . 118.6(5) ?
C15 C14 H14 . 120.7 ?
C13 C14 H14 . 120.7 ?
C14 C15 C10 . 122.8(5) ?
C14 C15 C16 . 133.2(5) ?
C10 C15 C16 . 103.8(5) ?
N4 C16 N3 . 128.2(5) ?
N4 C16 C15 . 122.2(5) ?
N3 C16 C15 . 109.5(4) ?
N4 C17 N5 . 127.0(5) ?
N4 C17 C18 . 124.2(5) ?
N5 C17 C18 . 108.7(5) ?
C23 C18 C19 . 118.7(5) ?
C23 C18 C17 . 109.2(5) ?
C19 C18 C17 . 132.1(5) ?
C20 C19 C18 . 118.3(5) ?
C20 C19 H19 . 120.9 ?
C18 C19 H19 . 120.9 ?
C19 C20 C21 . 120.5(5) ?
C19 C20 H20 . 119.8 ?
C21 C20 H20 . 119.8 ?
C22 C21 C20 . 123.0(5) ?
C22 C21 H21 . 118.5 ?
C20 C21 H21 . 118.5 ?
C21 C22 C23 . 115.8(5) ?
C21 C22 H22 . 122.1 ?
C23 C22 H22 . 122.1 ?
C18 C23 C22 . 123.7(5) ?
C18 C23 C24 . 105.3(5) ?
C22 C23 C24 . 131.0(5) ?
N6 C24 N5 . 127.7(5) ?
N6 C24 C23 . 122.7(5) ?
N5 C24 C23 . 109.6(5) ?
N6 C25 N7 . 125.4(5) ?
N6 C25 C26 . 123.8(5) ?
N7 C25 C26 . 110.6(4) ?
C27 C26 C25 . 134.3(5) ?
C27 C26 C31 . 119.2(5) ?
C25 C26 C31 . 106.0(5) ?
C28 C27 C26 . 121.3(6) ?
C28 C27 H27 . 119.3 ?
C26 C27 H27 . 119.3 ?
C27 C28 C29 . 120.0(6) ?
C27 C28 H28 . 120.0 ?
C29 C28 H28 . 120.0 ?
C30 C29 C28 . 120.7(6) ?
C30 C29 H29 . 119.6 ?
C28 C29 H29 . 119.6 ?
C31 C30 C29 . 119.7(6) ?
C31 C30 H30 . 120.1 ?
C29 C30 H30 . 120.1 ?
C30 C31 C32 . 134.1(6) ?
C30 C31 C26 . 118.8(5) ?
C32 C31 C26 . 107.1(5) ?
N8 C32 C31 . 124.2(5) ?
N8 C32 N7 . 125.9(5) ?
C31 C32 N7 . 109.9(5) ?
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 Mn1 . 2.7312(11) y
Mn1 N7 . 1.953(4) y
Mn1 N5 . 1.969(4) y
Mn1 N3 . 1.969(4) y
Mn1 N1 . 1.974(4) y
I2 I2 2_556 2.7827(12) y
I1 I2 . 3.4238(10) y
N1 C8 . 1.375(6) ?
N1 C1 . 1.408(6) ?
N2 C8 . 1.318(6) ?
N2 C9 . 1.337(6) ?
N3 C16 . 1.398(6) ?
N3 C9 . 1.401(6) ?
N4 C16 . 1.315(6) ?
N4 C17 . 1.343(6) ?
N5 C17 . 1.372(6) ?
N5 C24 . 1.395(6) ?
N6 C24 . 1.327(6) ?
N6 C25 . 1.329(6) ?
N7 C25 . 1.411(6) ?
N7 C32 . 1.421(6) ?
N8 C1 . 1.302(6) ?
N8 C32 . 1.331(6) ?
C1 C2 . 1.461(7) ?
C2 C3 . 1.414(7) ?
C2 C7 . 1.429(7) ?
C3 C4 . 1.364(7) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.362(7) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.402(7) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.323(7) ?
C6 H6 . 0.9300 ?
C7 C8 . 1.489(6) ?
C9 C10 . 1.428(7) ?
C10 C15 . 1.429(6) ?
C10 C11 . 1.434(7) ?
C11 C12 . 1.366(7) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.447(7) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.396(7) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.353(7) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.499(7) ?
C17 C18 . 1.454(7) ?
C18 C23 . 1.363(7) ?
C18 C19 . 1.423(7) ?
C19 C20 . 1.376(7) ?
C19 H19 . 0.9300 ?
C20 C21 . 1.388(7) ?
C20 H20 . 0.9300 ?
C21 C22 . 1.359(6) ?
C21 H21 . 0.9300 ?
C22 C23 . 1.406(7) ?
C22 H22 . 0.9300 ?
C23 C24 . 1.470(6) ?
C25 C26 . 1.421(7) ?
C26 C27 . 1.382(7) ?
C26 C31 . 1.458(7) ?
C27 C28 . 1.363(7) ?
C27 H27 . 0.9300 ?
C28 C29 . 1.407(7) ?
C28 H28 . 0.9300 ?
C29 C30 . 1.398(8) ?
C29 H29 . 0.9300 ?
C30 C31 . 1.390(7) ?
C30 H30 . 0.9300 ?
C31 C32 . 1.414(7) ?
