#------------------------------------------------------------------------------
#$Date: 2018-09-12 04:52:57 +0300 (Wed, 12 Sep 2018) $
#$Revision: 210872 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/26/2242631.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_2242631
loop_
_publ_author_name
'Lynch, Will'
'Lynch, Genevieve'
'Sheriff, Kirk'
'Padgett, Clifford'
_publ_section_title
;
 Structures of substituted pyridine N-oxide with manganese(II)
 acetate
;
_journal_coeditor_code           ZL2728
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1405
_journal_page_last               1410
_journal_paper_doi               10.1107/S205698901801232X
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Mn4 (C2 H3 O2)8 (C5 H5 N O)2 (H2 O)2]'
_chemical_formula_moiety         'C26 H38 Mn4 N2 O20'
_chemical_formula_sum            'C26 H38 Mn4 N2 O20'
_chemical_formula_weight         918.3396
_chemical_name_systematic
;catena-Poly[manganese(II)-μ₃-acetato-di-μ₂-acetato-[aquamanganese(II)]-μ₂-acetato-μ-(pyridine N-oxide)-manganese(II)-μ₃-acetato-μ₂-acetato-μ-(pyridine
N-oxide)-[aquamanganese(II)]-di-μ₂-acetato]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.925(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.936(7)
_cell_length_b                   10.603(4)
_cell_length_c                   18.692(7)
_cell_measurement_reflns_used    5012
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.1
_cell_volume                     3800(2)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2009)
;
_computing_molecular_graphics
;
OLEX2  (Dolomanov et al.,  2009)
;
_computing_publication_material
;
OLEX2  (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
ShelXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
ShelXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19620
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         2.125
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.378
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(REQAB; Rigaku, 1998)
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    "'not measured"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.362
_refine_ls_extinction_coef       0.00109(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/1 (Sheldrick 2015)
;
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4332
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0348P)²+3.1638P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                3855
_reflns_number_total             4332
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            zl2728sup1.cif
_cod_data_source_block           I
_cod_database_code               2242631
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.609
_shelx_estimated_absorpt_t_max   0.770
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_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_occupancy
Mn Mn1 0.500000 0.500000 0.500000 0.02291(11) Uani d 1
O O1 0.60564(7) 0.50006(13) 0.57232(8) 0.0254(3) Uani d 1
C C1 0.60680(13) 0.5206(2) 0.69567(13) 0.0368(5) Uani d 1
H H1 0.594602 0.605051 0.687011 0.044 Uiso calc 1
N N1 0.61602(8) 0.44789(16) 0.64043(9) 0.0226(3) Uani d 1
Mn Mn2 0.68359(2) 0.53844(3) 0.51070(2) 0.01989(10) Uani d 1
C C2 0.61555(15) 0.4693(3) 0.76534(13) 0.0455(6) Uani d 1
H H2 0.609182 0.519044 0.803946 0.055 Uiso calc 1
O O2 0.45997(7) 0.59052(14) 0.58476(8) 0.0290(3) Uani d 1
O O3 0.34900(7) 0.64803(13) 0.54422(8) 0.0251(3) Uani d 1
C C3 0.63378(13) 0.3441(2) 0.77773(13) 0.0398(6) Uani d 1
H H3 0.640102 0.308856 0.824684 0.048 Uiso calc 1
Mn Mn3 0.750000 0.250000 0.500000 0.02146(11) Uani d 1
C C4 0.64253(12) 0.2717(2) 0.71959(13) 0.0355(5) Uani d 1
H H4 0.654963 0.187201 0.727123 0.043 Uiso calc 1
O O4 0.51209(8) 0.68135(14) 0.45732(9) 0.0319(3) Uani d 1
O O5 0.62046(8) 0.67838(14) 0.44529(8) 0.0287(3) Uani d 1
C C5 0.63271(11) 0.3254(2) 0.65014(12) 0.0280(4) Uani d 1
H H5 0.637647 0.276949 0.610427 0.034 Uiso calc 1
C C6 0.41374(10) 0.67368(19) 0.57075(11) 0.0241(4) Uani d 1
O O6 0.75532(7) 0.56777(13) 0.44447(8) 0.0269(3) Uani d 1
C C7 0.43584(13) 0.8095(2) 0.58470(15) 0.0402(6) Uani d 1
H H7A 0.459117 0.836106 0.548603 0.060 Uiso calc 1
H H7B 0.467028 0.817737 0.633739 0.060 Uiso calc 1
H H7C 0.395451 0.861292 0.580629 0.060 Uiso calc 1
O O7 0.79968(8) 0.37538(13) 0.44121(8) 0.0299(3) Uani d 1
O O8 0.74244(7) 0.10035(13) 0.41514(7) 0.0239(3) Uani d 1
C C8 0.56142(11) 0.72708(19) 0.43642(12) 0.0268(4) Uani d 1
C C9 0.54817(15) 0.8513(3) 0.39541(19) 0.0567(8) Uani d 1
H H9A 0.520255 0.837263 0.345358 0.085 Uiso calc 1
H H9C 0.591852 0.888472 0.394560 0.085 Uiso calc 1
H H9B 0.523979 0.907121 0.420264 0.085 Uiso calc 1
O O9 0.69630(12) -0.01467(16) 0.31454(10) 0.0552(6) Uani d 1
C C10 0.79817(10) 0.49193(19) 0.42916(11) 0.0235(4) Uani d 1
O O10 0.72800(9) 0.68131(14) 0.59148(9) 0.0324(3) Uani d 1
H H10A 0.7598(12) 0.645(3) 0.6246(13) 0.049 Uiso d 1
H H10B 0.7398(15) 0.7520(19) 0.5805(16) 0.049 Uiso d 1
C C11 0.85076(14) 0.5440(2) 0.39252(16) 0.0435(6) Uani d 1
H H11A 0.833091 0.536035 0.339502 0.065 Uiso calc 1
H H11B 0.893627 0.497746 0.409250 0.065 Uiso calc 1
H H11C 0.859103 0.631314 0.405432 0.065 Uiso calc 1
C C12 0.70807(11) 0.0878(2) 0.34617(11) 0.0286(4) Uani d 1
C C13 0.68183(13) 0.2058(2) 0.30226(12) 0.0362(5) Uani d 1
H H13A 0.691076 0.277449 0.334898 0.054 Uiso calc 1
H H13B 0.632510 0.198775 0.279886 0.054 Uiso calc 1
H H13C 0.705221 0.216242 0.264085 0.054 Uiso calc 1
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'
O O 0.0106 0.0060 '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
O1 Mn1 O1 5_666 . 180.00(7)
O1 Mn1 O2 5_666 5_666 91.91(6)
O1 Mn1 O2 . 5_666 88.09(6)
O1 Mn1 O2 5_666 . 88.09(6)
O1 Mn1 O2 . . 91.91(6)
O2 Mn1 O2 . 5_666 180.0
O4 Mn1 O1 5_666 5_666 92.47(6)
O4 Mn1 O1 . . 92.47(6)
O4 Mn1 O1 5_666 . 87.53(6)
O4 Mn1 O1 . 5_666 87.53(6)
O4 Mn1 O2 5_666 . 91.36(6)
O4 Mn1 O2 . . 88.64(6)
O4 Mn1 O2 . 5_666 91.36(6)
O4 Mn1 O2 5_666 5_666 88.64(6)
O4 Mn1 O4 . 5_666 180.0
Mn1 O1 Mn2 . . 112.12(6)
N1 O1 Mn1 . . 117.31(11)
N1 O1 Mn2 . . 128.21(11)
N1 C1 H1 . . 120.3
N1 C1 C2 . . 119.5(2)
C2 C1 H1 . . 120.3
C1 N1 O1 . . 118.17(18)
C5 N1 O1 . . 119.51(16)
C5 N1 C1 . . 122.28(19)
O1 Mn2 O3 . 5_666 85.37(6)
O1 Mn2 O8 . 7_656 89.66(5)
O3 Mn2 O8 5_666 7_656 76.44(5)
O5 Mn2 O1 . . 92.21(6)
O5 Mn2 O3 . 5_666 107.68(6)
O5 Mn2 O6 . . 87.13(6)
O5 Mn2 O8 . 7_656 175.59(6)
O5 Mn2 O10 . . 88.66(6)
O6 Mn2 O1 . . 176.02(6)
O6 Mn2 O3 . 5_666 91.08(6)
O6 Mn2 O8 . 7_656 91.27(6)
O10 Mn2 O1 . . 88.66(6)
O10 Mn2 O3 . 5_666 162.77(6)
O10 Mn2 O6 . . 95.25(6)
O10 Mn2 O8 . 7_656 87.39(6)
C1 C2 H2 . . 120.1
C1 C2 C3 . . 119.9(2)
C3 C2 H2 . . 120.1
C6 O2 Mn1 . . 123.62(13)
Mn3 O3 Mn2 3_455 5_666 98.27(6)
C6 O3 Mn2 . 5_666 120.04(12)
C6 O3 Mn3 . 3_455 138.28(13)
C2 C3 H3 . . 120.4
C2 C3 C4 . . 119.2(2)
C4 C3 H3 . . 120.4
O3 Mn3 O3 5_666 3_545 180.00(7)
O3 Mn3 O8 5_666 7_656 78.19(5)
O3 Mn3 O8 3_545 7_656 101.81(5)
O3 Mn3 O8 3_545 . 78.19(5)
O3 Mn3 O8 5_666 . 101.81(5)
O7 Mn3 O3 . 5_666 89.75(6)
O7 Mn3 O3 7_656 3_545 89.75(6)
O7 Mn3 O3 7_656 5_666 90.25(6)
O7 Mn3 O3 . 3_545 90.25(6)
O7 Mn3 O7 . 7_656 180.0
O7 Mn3 O8 . . 91.58(6)
O7 Mn3 O8 . 7_656 88.43(6)
O7 Mn3 O8 7_656 7_656 91.57(6)
O7 Mn3 O8 7_656 . 88.43(6)
O8 Mn3 O8 . 7_656 180.00(5)
C3 C4 H4 . . 120.2
C3 C4 C5 . . 119.7(2)
C5 C4 H4 . . 120.2
C8 O4 Mn1 . . 130.47(13)
C8 O5 Mn2 . . 139.17(14)
N1 C5 C4 . . 119.5(2)
N1 C5 H5 . . 120.2
C4 C5 H5 . . 120.2
O2 C6 O3 . . 122.61(19)
O2 C6 C7 . . 118.29(19)
O3 C6 C7 . . 119.09(18)
C10 O6 Mn2 . . 129.45(13)
C6 C7 H7A . . 109.5
C6 C7 H7B . . 109.5
C6 C7 H7C . . 109.5
H7A C7 H7B . . 109.5
H7A C7 H7C . . 109.5
H7B C7 H7C . . 109.5
C10 O7 Mn3 . . 135.59(13)
Mn3 O8 Mn2 . 7_656 97.00(6)
C12 O8 Mn2 . 7_656 128.45(13)
C12 O8 Mn3 . . 134.54(13)
O4 C8 O5 . . 126.06(19)
O4 C8 C9 . . 116.96(19)
O5 C8 C9 . . 116.97(19)
C8 C9 H9A . . 109.5
C8 C9 H9C . . 109.5
C8 C9 H9B . . 109.5
H9A C9 H9C . . 109.5
H9A C9 H9B . . 109.5
H9C C9 H9B . . 109.5
O6 C10 C11 . . 117.96(18)
O7 C10 O6 . . 124.82(19)
O7 C10 C11 . . 117.21(18)
Mn2 O10 H10A . . 106(2)
Mn2 O10 H10B . . 124(2)
H10A O10 H10B . . 113(3)
C10 C11 H11A . . 109.5
C10 C11 H11B . . 109.5
C10 C11 H11C . . 109.5
H11A C11 H11B . . 109.5
H11A C11 H11C . . 109.5
H11B C11 H11C . . 109.5
O8 C12 C13 . . 117.86(18)
O9 C12 O8 . . 123.5(2)
O9 C12 C13 . . 118.66(19)
C12 C13 H13A . . 109.5
C12 C13 H13B . . 109.5
C12 C13 H13C . . 109.5
H13A C13 H13B . . 109.5
H13A C13 H13C . . 109.5
H13B C13 H13C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mn1 O1 5_666 2.1680(15)
Mn1 O1 . 2.1681(15)
Mn1 O2 5_666 2.1822(15)
Mn1 O2 . 2.1822(15)
Mn1 O4 5_666 2.1207(16)
Mn1 O4 . 2.1207(16)
O1 N1 . 1.351(2)
O1 Mn2 . 2.2113(15)
C1 H1 . 0.9300
C1 N1 . 1.341(3)
C1 C2 . 1.377(3)
N1 C5 . 1.341(3)
Mn2 O3 5_666 2.2404(15)
Mn2 O5 . 2.1062(15)
Mn2 O6 . 2.1551(15)
Mn2 O8 7_656 2.2671(14)
Mn2 O10 . 2.1506(16)
C2 H2 . 0.9300
C2 C3 . 1.380(4)
O2 C6 . 1.250(2)
O3 Mn3 3_455 2.2028(15)
O3 C6 . 1.278(2)
C3 H3 . 0.9300
C3 C4 . 1.380(3)
Mn3 O7 7_656 2.1338(15)
Mn3 O7 . 2.1338(15)
Mn3 O8 . 2.2194(14)
Mn3 O8 7_656 2.2194(14)
C4 H4 . 0.9300
C4 C5 . 1.381(3)
O4 C8 . 1.251(3)
O5 C8 . 1.254(2)
C5 H5 . 0.9300
C6 C7 . 1.508(3)
O6 C10 . 1.262(2)
C7 H7A . 0.9600
C7 H7B . 0.9600
C7 H7C . 0.9600
O7 C10 . 1.255(2)
O8 C12 . 1.290(2)
C8 C9 . 1.510(3)
C9 H9A . 0.9600
C9 H9C . 0.9600
C9 H9B . 0.9600
O9 C12 . 1.228(3)
C10 C11 . 1.506(3)
O10 H10A . 0.848(17)
O10 H10B . 0.829(17)
C11 H11A . 0.9600
C11 H11B . 0.9600
C11 H11C . 0.9600
C12 C13 . 1.509(3)
C13 H13A . 0.9600
C13 H13B . 0.9600
C13 H13C . 0.9600
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
O10 H10A O9 7_656 0.848(17) 1.85(2) 2.652(2) 157(3) yes
O10 H10B O6 7_666 0.829(17) 1.976(18) 2.786(2) 166(3) yes

_cod_database_fobs_code 2242631
