#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/42/2014215.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_2014215
loop_
_publ_author_name
'Bian, Guo-Qing'
'Kuroda-Sowa, Takayoshi'
'Konaka, Hisashi'
'Maekawa, Masahiko'
'Munakata, Megumu'
_publ_section_title
;
 Bis(μ-6-hydroxypicolinato)-μ-oxo-bis[dipyridinemanganese(III)]
 monohydrate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m338
_journal_page_last               m340
_journal_paper_doi               10.1107/S0108270104012624
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Mn2 O (C6 H3 N O3)2 (C5 H5 N)4], H2 O'
_chemical_formula_moiety         'C32 H26 Mn2 N6 O7, H2 O'
_chemical_formula_sum            'C32 H28 Mn2 N6 O8'
_chemical_formula_weight         734.48
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 104.118(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.606(8)
_cell_length_b                   16.379(9)
_cell_length_c                   14.289(9)
_cell_measurement_reflns_used    4653
_cell_measurement_temperature    150.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3088(3)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       'CRYSTALCLEAR (Rigaku, 2001)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation & Rigaku, 2000)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11903
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1504.0
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.46
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3144
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.0468P)²+5.1887P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                3144
_reflns_number_total             3512
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ob1180.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-c 2yc'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2014215
_cod_database_fobs_code          2014215
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y,1/2-z
-x,-y,-z
x,-y,1/2+z
1/2+x,1/2+y,z
1/2-x,1/2+y,1/2-z
1/2-x,1/2-y,-z
1/2+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
Mn1 0.58631(3) 0.16515(2) 0.19278(2) 0.02280(10) Uani d . 1.00 . . Mn
O1 0.51920(10) 0.08470(10) 0.38860(10) 0.0297(4) Uani d . 1.00 . . O
O2 0.69320(10) 0.11810(10) 0.14170(10) 0.0268(4) Uani d . 1.00 . . O
O3 0.8395(2) 0.05210(10) 0.18210(10) 0.0427(5) Uani d . 1.00 . . O
O4 0.5000 0.21560(10) 0.2500 0.0252(5) Uani d S 1.00 . . O
O5 1.0000 0.0515(2) 0.7500 0.0424(7) Uani d S 1.00 . . O
N1 0.6409(2) 0.07840(10) 0.30060(10) 0.0240(4) Uani d . 1.00 . . N
N2 0.5556(2) 0.25230(10) 0.07500(10) 0.0257(4) Uani d . 1.00 . . N
N3 0.7118(2) 0.25550(10) 0.26990(10) 0.0283(4) Uani d . 1.00 . . N
C1 0.6019(2) 0.05480(10) 0.3756(2) 0.0253(5) Uani d . 1.00 . . C
C2 0.6569(2) -0.0049(2) 0.4417(2) 0.0285(5) Uani d . 1.00 . . C
C3 0.7470(2) -0.0340(2) 0.4319(2) 0.0308(5) Uani d . 1.00 . . C
C4 0.7860(2) -0.0089(2) 0.3537(2) 0.0300(5) Uani d . 1.00 . . C
C5 0.7297(2) 0.04590(10) 0.2898(2) 0.0253(5) Uani d . 1.00 . . C
C6 0.7594(2) 0.0728(2) 0.1992(2) 0.0277(5) Uani d . 1.00 . . C
C7 0.5118(2) 0.3234(2) 0.0869(2) 0.0310(6) Uani d . 1.00 . . C
C8 0.4805(2) 0.3789(2) 0.0126(2) 0.0366(6) Uani d . 1.00 . . C
C9 0.4965(2) 0.3616(2) -0.0768(2) 0.0368(6) Uani d . 1.00 . . C
C10 0.5439(2) 0.2896(2) -0.0888(2) 0.0379(6) Uani d . 1.00 . . C
C11 0.5720(2) 0.2362(2) -0.0120(2) 0.0311(5) Uani d . 1.00 . . C
C12 0.7163(2) 0.2782(2) 0.3605(2) 0.0405(7) Uani d . 1.00 . . C
C13 0.7876(3) 0.3334(2) 0.4094(2) 0.0524(9) Uani d . 1.00 . . C
C14 0.8557(2) 0.3672(2) 0.3655(2) 0.0457(7) Uani d . 1.00 . . C
C15 0.8516(2) 0.3444(2) 0.2713(2) 0.0402(6) Uani d . 1.00 . . C
C16 0.7793(2) 0.2884(2) 0.2269(2) 0.0339(6) Uani d . 1.00 . . C
H1 0.626(2) -0.0220(10) 0.492(2) 0.0146 Uiso d . 1.00 . . H
H2 0.783(2) -0.0690(10) 0.472(2) 0.0146 Uiso d . 1.00 . . H
H3 0.845(2) -0.0310(10) 0.343(2) 0.0146 Uiso d . 1.00 . . H
H4 0.502(2) 0.3350(10) 0.147(2) 0.0146 Uiso d . 1.00 . . H
H5 0.452(2) 0.425(2) 0.027(2) 0.0146 Uiso d . 1.00 . . H
H6 0.478(2) 0.3980(10) -0.128(2) 0.0146 Uiso d . 1.00 . . H
H7 0.553(2) 0.2740(10) -0.149(2) 0.0146 Uiso d . 1.00 . . H
H8 0.604(2) 0.188(2) -0.018(2) 0.0146 Uiso d . 1.00 . . H
H9 0.667(2) 0.2490(10) 0.390(2) 0.0146 Uiso d . 1.00 . . H
H10 0.786(2) 0.3460(10) 0.463(2) 0.0146 Uiso d . 1.00 . . H
H11 0.906(2) 0.4060(10) 0.396(2) 0.0146 Uiso d . 1.00 . . H
H12 0.894(2) 0.3670(10) 0.239(2) 0.0146 Uiso d . 1.00 . . H
H13 0.774(2) 0.2710(10) 0.165(2) 0.0146 Uiso d . 1.00 . . H
H14 1.050(2) 0.0180(10) 0.772(2) 0.0146 Uiso d . 1.00 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
Mn Mn 0.337 0.728
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, 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
O1 Mn1 O2 2_655 . 90.95(8) y
O1 Mn1 O4 2_655 . 96.18(8) y
O1 Mn1 N1 2_655 . 93.10(7) y
O1 Mn1 N2 2_655 . 90.41(7) y
O1 Mn1 N3 2_655 . 173.97(8) yes
O2 Mn1 O4 . . 172.80(6) yes
O2 Mn1 N1 . . 80.98(8) y
O2 Mn1 N2 . . 89.37(8) y
O2 Mn1 N3 . . 84.24(8) y
O4 Mn1 N1 . . 97.59(7) y
O4 Mn1 N2 . . 91.55(8) y
O4 Mn1 N3 . . 88.71(8) y
N1 Mn1 N2 . . 169.78(9) yes
N1 Mn1 N3 . . 89.75(7) y
N2 Mn1 N3 . . 85.91(7) y
Mn1 O1 C1 2_655 . 132.1(2) n
Mn1 O2 C6 . . 117.3(2) n
Mn1 O4 Mn1 . 2_655 125.00(10) yes
Mn1 N1 C1 . . 129.4(2) n
Mn1 N1 C5 . . 110.3(2) n
C1 N1 C5 . . 120.2(2) n
Mn1 N2 C7 . . 118.8(2) n
Mn1 N2 C11 . . 123.1(2) n
C7 N2 C11 . . 118.0(2) n
Mn1 N3 C12 . . 119.4(2) n
Mn1 N3 C16 . . 123.1(2) n
C12 N3 C16 . . 117.4(2) n
O1 C1 N1 . . 122.0(2) n
O1 C1 C2 . . 119.9(2) n
N1 C1 C2 . . 118.1(2) n
C1 C2 C3 . . 120.7(2) n
C2 C3 C4 . . 120.3(2) n
C3 C4 C5 . . 117.5(3) n
N1 C5 C4 . . 123.1(2) n
N1 C5 C6 . . 114.3(2) n
C4 C5 C6 . . 122.6(2) n
O2 C6 O3 . . 123.3(2) n
O2 C6 C5 . . 114.9(2) n
O3 C6 C5 . . 121.8(2) n
N2 C7 C8 . . 122.5(3) n
C7 C8 C9 . . 119.2(3) n
C8 C9 C10 . . 118.6(3) n
C9 C10 C11 . . 119.3(3) n
N2 C11 C10 . . 122.4(3) n
N3 C12 C13 . . 122.2(3) n
C12 C13 C14 . . 120.4(3) n
C13 C14 C15 . . 117.9(3) n
C14 C15 C16 . . 118.8(3) n
N3 C16 C15 . . 123.3(3) n
H14 O5 H14 . 2_756 102(2) no
C1 C2 H1 . . 116.0(10) no
C3 C2 H1 . . 123.0(10) no
C2 C3 H2 . . 122.0(10) no
C4 C3 H2 . . 116.0(10) no
C3 C4 H3 . . 121.0(10) no
C5 C4 H3 . . 120.0(10) no
N2 C7 H4 . . 118.0(10) no
C8 C7 H4 . . 119.0(10) no
C7 C8 H5 . . 116.0(10) no
C9 C8 H5 . . 124.0(10) no
C8 C9 H6 . . 121.0(10) no
C10 C9 H6 . . 119.0(10) no
C9 C10 H7 . . 121.0(10) no
C11 C10 H7 . . 119.0(10) no
N2 C11 H8 . . 116.0(10) no
C10 C11 H8 . . 121.0(10) no
N3 C12 H9 . . 113.0(10) no
C13 C12 H9 . . 124.0(10) no
C12 C13 H10 . . 118.0(10) no
C14 C13 H10 . . 121.0(10) no
C13 C14 H11 . . 123.0(10) no
C15 C14 H11 . . 118.0(10) no
C14 C15 H12 . . 120.0(10) no
C16 C15 H12 . . 120.0(10) no
N3 C16 H13 . . 114.0(10) no
C15 C16 H13 . . 122.0(10) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 Mn1 . 2_655 3.1720(10) yes
Mn1 O1 . 2_655 2.083(2) yes
Mn1 O2 . . 1.939(2) yes
Mn1 O4 . . 1.7890(10) yes
Mn1 N1 . . 2.094(2) yes
Mn1 N2 . . 2.169(2) yes
Mn1 N3 . . 2.325(2) yes
O1 C1 . . 1.282(3) n
O2 C6 . . 1.295(3) n
O3 C6 . . 1.222(4) n
N1 C1 . . 1.363(3) n
N1 C5 . . 1.363(3) n
N2 C7 . . 1.338(3) n
N2 C11 . . 1.341(3) n
N3 C12 . . 1.334(4) n
N3 C16 . . 1.336(4) n
C1 C2 . . 1.437(3) n
C2 C3 . . 1.354(4) n
C3 C4 . . 1.410(4) n
C4 C5 . . 1.373(3) n
C5 C6 . . 1.513(4) n
C7 C8 . . 1.384(4) n
C8 C9 . . 1.377(4) n
C9 C10 . . 1.375(4) n
C10 C11 . . 1.382(4) n
C12 C13 . . 1.384(4) n
C13 C14 . . 1.358(5) n
C14 C15 . . 1.385(5) n
C15 C16 . . 1.380(4) n
O5 H14 . . 0.87(2) no
O5 H14 . 2_756 0.87(2) no
C2 H1 . . 0.96(3) no
C3 H2 . . 0.87(2) no
C4 H3 . . 0.93(3) no
C7 H4 . . 0.92(3) no
C8 H5 . . 0.90(3) no
C9 H6 . . 0.93(2) no
C10 H7 . . 0.93(3) no
C11 H8 . . 0.92(3) no
C12 H9 . . 1.00(3) no
C13 H10 . . 0.80(3) no
C14 H11 . . 0.96(2) no
C15 H12 . . 0.90(3) no
C16 H13 . . 0.92(3) no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
O1 C14 3.597(3) 7_656
O2 C2 3.340(3) 4_554
O2 C3 3.534(3) 4_554
O3 O5 2.748(3) 3_756
O3 C9 3.298(4) 7_655
O3 C10 3.471(4) 7_655
O3 C3 3.500(3) 4_554
O5 C7 3.137(3) 7_656
O5 C7 3.137(3) 8_555
O5 C8 3.526(3) 7_656
O5 C8 3.526(3) 8_555
C1 C13 3.578(4) 7_656
C2 C13 3.494(4) 7_656
C2 C14 3.596(4) 7_656
C3 C15 3.507(4) 6_645
C4 C15 3.292(4) 6_645
C4 C16 3.555(4) 6_645
C5 C15 3.522(4) 6_645
C10 C14 3.572(4) 8_454
C11 C14 3.476(4) 8_454
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O5 H14 O3 3_756 0.87(2) 1.88(2) 2.748(3) 178.0(10) y
C2 H1 O2 4_555 0.96(3) 2.63(2) 3.340(3) 131(2) y
C7 H4 O5 7_656 0.92(3) 2.38(2) 3.137(3) 140(2) y
